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1-Pyrrolidinamine → HCID 57970128、化合物

HRID 1666611
ノート
印刷プレビュー

反応式

HRID 1666611 の反応式
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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 279461-PyrrolidinamineHCID 693814-MethylpiperidineHCID 81531DiisopropylethylamineHCID 12504008HCID 12504008、化合物HCID 86636479(S)-1-(3-aminopyrrolidin-1-yl)-2-(4-trifluoromethoxyphenyl)ethanone mono hydrochloride

生成物 1

HCID 57970128HCID 57970128、化合物収率 3%

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

反応条件

温度
110 °C

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-7ab834c923084f9597ce6439b0571492
出典データセット
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08044068B2

反応ノート

読み込み中…

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