Synthesis of small 3-fluoro- and 3,3-difluoropyrrolidines using azomethine ylide chemistry
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1 Synthesis of small 3-fluoro- and 3,3-difluoropyrrolidines using azomethine ylide chemistry Indrawan McAlpine*, Michelle Tran-Dubé, en Wang, Stephanie Scales, Jean Matthews, Michael R. Collins, Sajiv K. air, Mary guyen, Jianwei Bian, Luis Martinez Alsina, Jianmin Sun, Jiaying Zhong, Joseph S. Warmus, Brian T. eill Pfizer Worldwide Medicinal Chemistry, Pfizer Research & Development, Science Center Drive, San Diego CA Pfizer Worldwide Medicinal Chemistry, Pfizer Research & Development, 445 Eastern Point Road, Groton, CT Supporting information Content HRMS experimental..s1 1 HMR, 13 CMR, and 19 MR.S2 High Resolution Mass Method All data were gathered on an Agilent 1290 LC connected to Agilent T model G6230B with Atmospheric Pressure Chemical Ionization source. Elution Conditions: Column: WatersAcquityBEH C18, 2.1x30mm, 1.7µm particle size; Column Temperature 80 C Solvent A: Water (0.1% formic acid % ammonium formate) Solvent B: Acetonitrile (5%H2+0.1% formic acid+0.05% ammonium formate) Gradient: 5-95 %B in 2.5 min, 95%B min; low rate 1.2 ml/min, Injection Volume 1µL MSD Conditions: APCI source in positive ionization mode in profile mode was used. The spray chamber: Drying gas flow 6 L/min, ebulizer Pressure 50 psig, Drying gas temperature 325 C, Capillary Voltage 3500 V, Capillary current µa, Chamber µa, ragmentor 80 volt, Skimmer at 65 volt and CT 1 R Vpp 750 V. The acquisition done in scan mode with range of amu with acquisition rate of 10 spectra per second and transient/spectrum 895. Two internal references compounds of 121 amu and 922 amu was infused to source at all time during the analysis for instrument calibration verification S1
2 S diethyl (3R,4S)-1-benzyl-3-fluoropyrrolidine-3,4-dicarboxylate 2 1 HMR, CDCl 3, 400 MHz
3 diethyl (3R,4S)-1-benzyl-3-fluoropyrrolidine-3,4-dicarboxylate H CMR, CDCl 3, 101 MHz diethyl (3R,4S)-1-benzyl-3-fluoropyrrolidine-3,4-dicarboxylate 2 1 MR, CDCl 3, 376 MHz S3
4 S ethyl (3R,4R)-1-benzyl-3-fluoro-4-phenylpyrrolidine-3-carboxylate 3 1 HMR, CDCl 3, 400 MHz
5 S ethyl (3R,4R)-1-benzyl-3-fluoro-4-phenylpyrrolidine-3-carboxylate 3 13 CMR, CDCl 3, 101 MHz
6 ethyl (3R,4R)-1-benzyl-3-fluoro-4-phenylpyrrolidine-3-carboxylate 3 19 MR, CDCl 3, 376 MHz S6
7 CHLRRM-d benzyl 3,3,3-trifluoropropanoate (5a) C 5a 1 H MR, CDCl 3, 400MHz CHLRRM-d C 5a C MR, CDCl 3, 101 MHz S7
8 benzyl 3,3,3-trifluoropropanoate (5a) M01(s) a 19 MR, CDCl 3, 376 MHz S8
9 CHLRRM-d 5.23 SM a 1 H MR, CDCl 3, 400 MHz Benzyl 3,3-difluoroacrylate (6a) a 13 C MR, CDCl 3, 101 MHz CHLRRM-d S9
10 Benzyl 3,3-difluoroacrylate (6a). SM a 19 MR, CDCl 3, 376 MHz S10
11 7.37 benzyl 1-benzyl-4,4-difluoropyrrolidine-3-carboxylate (7a) Bn Bn 7a 1 H MR, CDCl 3, 400 MHz CHLRRM-d benzyl 1-benzyl-4,4-difluoropyrrolidine-3-carboxylate (7a) CHLRRM-d Bn Bn 7a 13 C MR, CDCl 3, 101 MHz S11
12 benzyl 1-benzyl-4,4-difluoropyrrolidine-3-carboxylate (7a) 7a 19 MR, CDCl 3, 376 MHz S12
13 7.33 ethyl 1-benzyl-4,4-difluoropyrrolidine-3-carboxylate (7b) b 1 H MR, CDCl 3, 400 MHz CHLRRM-d CHLRRM-d b C MR, CDCl 3, 101MHz S13
14 ethyl 1-benzyl-4,4-difluoropyrrolidine-3-carboxylate (7b) b 19 MR, CDCl 3, 376 MHz S14
15 1-(tert-butoxycarbonyl)-4,4-difluoropyrrolidine-3-carboxylic acid (8a) 1.43 H 8a 1 H MR, DMS-d 6, 400 MHz 3.75 DMS-d DMS-d6 1-(tert-butoxycarbonyl)-4,4-difluoropyrrolidine-3-carboxylic acid (8a) H 8a 13 C, DMS-d 6, 101 MHz, 80 C S15
16 (tert-butoxycarbonyl)-4,4-difluoropyrrolidine-3-carboxylic acid (8a) H 8a 19 MR, DMS-d 6, 376 MHz, 80 C S16
17 1-(tert-butyl) 3-ethyl 4,4-difluoropyrrolidine-1,3-dicarboxylate (8b) b 1 H MR, CDCl 3, 400 MHz CHLRRM-d (tert-butyl) 3-ethyl 4,4-difluoropyrrolidine-1,3-dicarboxylate (8b) CHLRRM-d b 13 C MR, CDCl 3, 101 MHz S17
18 1-(tert-butyl) 3-ethyl 4,4-difluoropyrrolidine-1,3-dicarboxylate (8b) b 19 MR, CDCl 3, 376 MHz S18
19 DMS-d tert-butyl 3,3-difluoro-4-(hydroxymethyl)pyrrolidine-1-carboxylate (9) H 9 1 H MR, DMS-d 6, 400 MHz DMS-d6 tert-butyl 3,3-difluoro-4-(hydroxymethyl)pyrrolidine-1-carboxylate (9) 15 9 H 13 CMR, DMS-d 6, 101 MHz, 80 C S19
20 tert-butyl 3,3-difluoro-4-(hydroxymethyl)pyrrolidine-1-carboxylate (9) H 9 19 MR, DMS-d 6, 376 MHz, 100 C S20
21 M02(s) M01(s) M03(m) M04(s) benzyl-3-tert-butoxy-1H-pyrrole-2,5-dione 15 1 HMR, CDCl 3, 400 MHZ M11(s) benzyl-3-tert-butoxy-1H-pyrrole-2,5-dione M07(s) M06(s) M05(s) CMR, CDCl 3, 101 MHZ M08(s) M10(s) M09(s) M04(s) M01(s) M02(s) M03(s) S21
22 S M07(dd) M09(dd) M03(m) M06(d) M01(m) M02(m) M08(dd) M10(m) M05(m) M04(m) ,5-dibenzyl-3a-fluorotetrahydropyrrolo[3,4-c]pyrrole-1,3(2H,3aH)-dione H 1 HMR, CDCl 3, 400 MHz M14(s) M15(s) M16(s) M17(s) M13(s) M05(s) M04(s) M11(d) M09(s) M08(m) M01(d) M12(s) M03(s) M02(m) M10(d) M06(m) ,5-dibenzyl-3a-fluorotetrahydropyrrolo[3,4-c]pyrrole-1,3(2H,3aH)-dione 13 CMR, CDCl 3, 101 MHz H 16
23 M01(m) ,5-dibenzyl-3a-fluorotetrahydropyrrolo[3,4-c]pyrrole-1,3(2H,3aH)-dione H MR, CDCl 3, 376 MHz S23
24 M06(s) 1.43 tert-butyl 5-benzyl-3a-fluoro-4,6-dioxohexahydropyrrolo[3,4-c]pyrrole-2(1H)-carboxylate H 17 1 HMR, CDCl 3, 400 MHz M01(m) 7.32 M02(s) 4.70 M03(m) M04(m) M05(m) M14(s) tert-butyl 5-benzyl-3a-fluoro-4,6-dioxohexahydropyrrolo[3,4-c]pyrrole-2(1H)-carboxylate M05(s) M06(s) M07(s) H CMR, CDCl 3, 101 MHz M08(s) M12(s) M13(s) M02(m) M01(d) M03(s) M04(s) M09(m) M11(br. s.) M10(m) S24
25 tert-butyl 5-benzyl-3a-fluoro-4,6-dioxohexahydropyrrolo[3,4-c]pyrrole-2(1H)-carboxylate H MR, CDCl 3, 376 MHz M01(s) S25
26 M08(s) M02(m) 1.44 tert-butyl 5-benzyl-3a-fluorohexahydropyrrolo[3,4-c]pyrrole-2(1H)-carboxylate H 18 1 HMR, CDCl 3, 400 MHz M01(m) M03(m) M04(m) M05(dd) M06(m) M07(br. s.) M05(s) M03(s) M04(s) tert-butyl 5-benzyl-3a-fluorohexahydropyrrolo[3,4-c]pyrrole-2(1H)-carboxylate H M12(s) M06(s) M07(m) M13(br. s.) M08(s) M09(d) M01(s) M02(s) M14(br. s.) M10(br. s.) CMR, CDCl 3, 101 MHz S26
27 M01(br. s.) tert-butyl 5-benzyl-3a-fluorohexahydropyrrolo[3,4-c]pyrrole-2(1H)-carboxylate H MR, CDCl 3, 376 MHz S27
28 S H MR, CDCl 3, 400 MHz H 1-benzyl-4,4-difluoropyrrolidin-3-ol H 1-benzyl-4,4-difluoropyrrolidin-3-ol C MR, CDCl 3, 101 MHz
29 benzyl-4,4-difluoropyrrolidin-3-ol H MR, CDCl 3, 376 MHz S29
30 benzyl-4-(benzyloxy)-3,3-difluoropyrrolidine 21 1 HMR, CDCl 3, 400 MHz benzyl-4-(benzyloxy)-3,3-difluoropyrrolidine CMR, CDCl 3, 101 MHz S30
31 benzyl-4-(benzyloxy)-3,3-difluoropyrrolidine MR, CDCl 3, 376 MHz S31
32 S H MR, CDCl 3, 400 MHz S S 1-benzyl-4,4-difluoropyrrolidin-3-yl 4-methylbenzenesulfonate C MR, CDCl 3, 101 MHz
33 benzyl-4,4-difluoropyrrolidin-3-yl 4-methylbenzenesulfonate S MR, CDCl 3, 376 MHz S33
34 S Br 1-benzyl-4-(4-bromophenyl)-3,3-difluoropyrrolidine 25 1 HMR, CDCl 3, 400 MHz Br 1-benzyl-4-(4-bromophenyl)-3,3-difluoropyrrolidine CMR, CDCl 3, 101 MHz
35 1-benzyl-4-(4-bromophenyl)-3,3-difluoropyrrolidine -9 Br MR, CDCl 3, 376 MHz S35
36 TMS CHLRRM-d ,4-dichloro-2-(2,2-difluorovinyl)benzene (26b) Cl Cl 26b 1 H MR, CDCl 3, 400 MHz CHLRRM-d 1,4-dichloro-2-(2,2-difluorovinyl)benzene (26b) Cl Cl 26b 13 C MR, CDCl 3, 101 MHz S36
37 ,4-dichloro-2-(2,2-difluorovinyl)benzene (26b) Cl Cl 26b 19 MR, CDCl 3, 376 MHz S37
38 S Cl Cl 1-benzyl-4-(2,4-dichlorophenyl)-3,3-difluoropyrrolidine 27a 1 H MR, CDCl 3, 400 MHz Cl Cl 1-benzyl-4-(2,4-dichlorophenyl)-3,3-difluoropyrrolidine 27a 13 C MR, CDCl 3, 101 MHz
39 benzyl-4-(2,4-dichlorophenyl)-3,3-difluoropyrrolidine Cl Cl a 19 MR, CDCl 3, 376 MHz S39
40 CHLRRM-d benzyl-4-(2,5-dichlorophenyl)-3,3-difluoropyrrolidine (27b) Cl Cl 27b H MR, CDCl 3, 400 MHz CHLRRM-d benzyl-4-(2,5-dichlorophenyl)-3,3-difluoropyrrolidine (27b) Cl Cl b 13 C MR, CDCl 3, 101 MHz S40
41 benzyl-4-(2,5-dichlorophenyl)-3,3-difluoropyrrolidine (27b) Cl Cl b 19 MR, CDCl 3, 376 MHz S41
42 benzyl-3,3-difluoro-4-(3-nitrophenyl)pyrrolidine c 1 HMR, CDCl 3, 400 MHz benzyl-3,3-difluoro-4-(3-nitrophenyl)pyrrolidine c 13 CMR, CDCl 3, 400 MHz S42
43 benzyl-3,3-difluoro-4-(3-nitrophenyl)pyrrolidine 2 27c 19 MR, CDCl 3, 400 MHz S43
44 benzyl-3,3-difluoro-4-(p-tolyl)pyrrolidine 27d 1 HMR, CDCl 3, 400 MHz benzyl-3,3-difluoro-4-(p-tolyl)pyrrolidine 27d 13 CMR, CDCl 3, 400 MHz S44
45 benzyl-3,3-difluoro-4-(p-tolyl)pyrrolidine d 19 MR, CDCl 3, 400 MHz S45
46 S benzyl-3,3-difluoro-4-(4-methoxyphenyl)pyrrolidine 27e 1 H MR, CDCl 3, 400 MHz benzyl-3,3-difluoro-4-(4-methoxyphenyl)pyrrolidine 27e 13 C MR, CDCl 3, 101 MHz
47 1-benzyl-3,3-difluoro-4-(4-methoxyphenyl)pyrrolidine e 19 MR, CDCl 3, 376 MHz S47
48 TMS CHLRRM-d benzyl-4-(4-(tert-butyl)phenyl)-3,3-difluoropyrrolidine (27f) 27f 1 H MR, CDCl 3, 400 MHz benzyl-4-(4-(tert-butyl)phenyl)-3,3-difluoropyrrolidine (27f) f 13 C MR, CDCl 3, 101 MHz CHLRRM-d S48
49 S Me 5-(1-benzyl-4,4-difluoropyrrolidin-3-yl)-2-methoxypyridine 29 1 H MR, CDCl 3, 400 MHz Me 5-(1-benzyl-4,4-difluoropyrrolidin-3-yl)-2-methoxypyridine C MR, CDCl 3, 101 MHz
50 (1-benzyl-4,4-difluoropyrrolidin-3-yl)-2-methoxypyridine Me MR, CDCl 3, 376 MHz S50
51 5-(2,2-difluorovinyl)-2-methoxypyrimidine Me 30 1 H MR, CDCl 3, 400 MHz (2,2-difluorovinyl)-2-methoxypyrimidine Me C MR, CDCl 3, 101 MHz S51
52 (2,2-difluorovinyl)-2-methoxypyrimidine Me MR, CDCl 3, 376 MHz S52
53 S (1-benzyl-4,4-difluoropyrrolidin-3-yl)-2-methoxypyrimidine 31 1 HMR, CDCl 3, 400 MHz (1-benzyl-4,4-difluoropyrrolidin-3-yl)-2-methoxypyrimidine CMR, CDCl 3, 101 MHz
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