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1-Pyrrolidinamine → HCID 57970128, 화합물

HRID 1666611
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HRID 1666611 반응식
Cl[C:2]1[CH:7]=[C:6](Cl)[CH:5]=[C:4]([CH3:9])[N+:3]=1[O-].Cl.[NH2:12][C@H:13]1[CH2:17][CH2:16][N:15]([C:18](=[O:31])[CH2:19][C:20]2[CH:25]=[CH:24][C:23]([O:26][C:27]([F:30])([F:29])[F:28])=[CH:22][CH:21]=2)[CH2:14]1.NN1CCCC1.[CH3:38][CH:39]1[CH2:44][CH2:43][NH:42][CH2:41][CH2:40]1.C(N(CC)C(C)C)(C)C>C(O)CCC>[CH3:38][CH:39]1[CH2:44][CH2:43][N:42]([C:6]2[CH:5]=[C:4]([CH3:9])[N:3]=[C:2]([NH:12][C@H:13]3[CH2:17][CH2:16][N:15]([C:18](=[O:31])[CH2:19][C:20]4[CH:21]=[CH:22][C:23]([O:26][C:27]([F:28])([F:29])[F:30])=[CH:24][CH:25]=4)[CH2:14]3)[CH:7]=2)[CH2:41][CH2:40]1
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HCID 279461-PyrrolidinamineHCID 693814-MethylpiperidineHCID 81531DiisopropylethylamineHCID 12504008HCID 12504008, 화합물HCID 86636479(S)-1-(3-aminopyrrolidin-1-yl)-2-(4-trifluoromethoxyphenyl)ethanone mono hydrochloride

생성물 1

HCID 57970128HCID 57970128, 화합물수율 3%

시약·촉매·용매 1

HCID 2631-Butanol용매

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온도
110 °C

실험 절차

In the same manner as in Example 13 (1), 1-((S)-3-(4-chloro-6-methyl-1-oxypyridin-2-ylamino)pyrrolidin-1-yl)-2-(4-trifluoromethoxyphenyl)ethanone (0.64 g) was obtained from 2,4-dichloro-6-methylpyridin-1-oxide (0.50 g) and 1-((S)-3-aminopyrrolidin-1-yl)-2-(4-trifluoromethoxyphenyl)ethanone mono hydrochloride (1.1 g). (2) A mixture of 1-((S)-3-(4-chloro-6-methyl-1-oxypyridin-2-ylamino)pyrrolidin-1-yl)-2-(4-trifluoromethoxyphenyl)ethanone (300 mg), 4-methylpiperidine (0.30 g), N,N-diisopropylethylamine (0.40 mL), and n-butanol (0.60 mL) was heated at 110° C. for 15 h. The mixture was cooled to room temperature, then the solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (NH silica gel, ethyl acetate−ethyl acetate/methanol=10:1) to obtain the title compound (40 mg) and 1-((S)-3-(4,6′-dimethyl-1′-oxy-3,4,5,6-tetrahydro-2H-[1,4′]bipyridinyl-2′-ylamino)pyrrolidin-1-yl)-2-(4-trifluoromethoxyphenyl)ethanone (200 mg). (3) 1-((S)-3-(4,6′-Dimethyl-1′-oxy-3,4,5,6-tetrahydro-2H-[1,4′]bipyridinyl-2′-ylamino)pyrrolidin-1-yl)-2-(4-trifluoromethoxyphenyl)ethanone (200 mg) was dissolved in methanol (6 mL), followed by addition of 10% Pd—C (200 mg), and the mixture stirred overnight at 40° C. under hydrogen atmosphere. The catalyst was removed by Celite filtration, then the filtrate was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (NH silica gel, chloroform/methanol=10:1) to obtain the title compound (64 mg).

후처리

  1. temperatureThe mixture was cooled to room temperature
  2. customthe solvent was evaporated under reduced pressure
  3. customthe residue was purified by silica gel column chromatography (NH silica gel, ethyl acetate−ethyl acetate/methanol=10:1)

출처 및 근거

ORD 기록
ord-7ab834c923084f9597ce6439b0571492
출처 데이터셋
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08044068B2

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