ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

1-Pyrrolidinamine → HCID 86636478、化合物

HRID 1666600
ノート
印刷プレビュー

反応式

HRID 1666600 の反応式
NN1CCCC1.[CH3:7][N:8]([CH3:29])[C:9]([CH:11]1[CH2:16][CH2:15][N:14]([C:17]2[C:26]3[C:21](=[CH:22][C:23]([F:27])=[CH:24][CH:25]=3)[N:20]=[C:19]([Cl:28])[N:18]=2)[CH2:13][CH2:12]1)=[O:10].Cl.[NH2:31][C@H:32]1[CH2:36][CH2:35][N:34]([C:37](=[O:50])[CH2:38][C:39]2[CH:44]=[CH:43][C:42]([O:45][C:46]([F:49])([F:48])[F:47])=[CH:41][CH:40]=2)[CH2:33]1.C(N(CC)C(C)C)(C)C>C(Cl)(Cl)Cl.C(=O)([O-])O.[Na+].C(O)CCC>[ClH:28].[CH3:7][N:8]([CH3:29])[C:9]([CH:11]1[CH2:16][CH2:15][N:14]([C:17]2[C:26]3[C:21](=[CH:22][C:23]([F:27])=[CH:24][CH:25]=3)[N:20]=[C:19]([NH:31][C@H:32]3[CH2:36][CH2:35][N:34]([C:37](=[O:50])[CH2:38][C:39]4[CH:40]=[CH:41][C:42]([O:45][C:46]([F:47])([F:48])[F:49])=[CH:43][CH:44]=4)[CH2:33]3)[N:18]=2)[CH2:13][CH2:12]1)=[O:10]
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

8

反応物 4

HCID 279461-PyrrolidinamineHCID 81531DiisopropylethylamineHCID 57970126HCID 57970126、化合物HCID 86636479(S)-1-(3-aminopyrrolidin-1-yl)-2-(4-trifluoromethoxyphenyl)ethanone mono hydrochloride

生成物 1

HCID 86636478HCID 86636478、化合物収率 23.7%

試薬・触媒・溶媒 3

HCID 263
1-Butanol
溶媒
HCID 6212Chloroform溶媒
HCID 516892Sodium Bicarbonate溶媒

反応条件

温度
120 °C

実験手順

A mixture of 2,4-dichloro-7-fluoroquinazoline (250 mg), piperidine-4-carboxylic acid dimethylamide (189 mg), triethylamine (0.24 mL), THF (6 mL), and DMF (4 mL) was stirred at room temperature for 13 h. The reaction mixture was diluted with a mixture of chloroform and saturated aqueous sodium hydrogencarbonate, and then the aqueous layer was extracted 3 times with chloroform. The organic layer was dried with anhydrous sodium sulfate, the desiccant was removed by filtration, the filtrate was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (hexane/ethyl acetate=7:3) to obtain colorless solid 1-(2-chloro-7-fluoroquinazolin-4-yl)piperidine-4-carboxylic acid dimethylamide (407 mg). (2) A mixture of 1-(2-chloro-7-fluoroquinazolin-4-yl)piperidine-4-carboxylic acid dimethylamide (250 mg), 1-((S)-3-aminopyrrolidin-1-yl)-2-(4-trifluoromethoxyphenyl)ethanone mono hydrochloride (265 mg), N,N-diisopropylethylamine (0.32 mL), and n-butanol (1.2 mL) was heated at 120° C. for 57 h with stirring. The reaction mixture was diluted with a mixture of chloroform and saturated aqueous sodium hydrogencarbonate, and then the aqueous layer was extracted with chloroform. The organic layer was dried with anhydrous sodium sulfate, the desiccant was removed by filtration, the filtrate was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (NH silica gel, hexane/ethyl acetate=4:1−ethyl acetate, and silica gel, chloroform/methanol=95:5). The resulting purification product was dissolved in ethyl acetate (2.0 mL), followed by addition of a solution (0.1 mL) of 4 M HCl in ethyl acetate, and the mixture was stirred at room temperature for 3.5 h. The solvent was evaporated under reduced pressure to obtain the amorphous title compound (110 mg).

後処理

  1. extractionthe aqueous layer was extracted with chloroform
  2. dry with materialThe organic layer was dried with anhydrous sodium sulfate
  3. customthe desiccant was removed by filtration
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. customthe residue was purified by silica gel column chromatography (NH silica gel, hexane/ethyl acetate=4:1−ethyl acetate, and silica gel, chloroform/methanol=95:5)
  6. customThe resulting purification product
  7. dissolutionwas dissolved in ethyl acetate (2.0 mL)
  8. additionfollowed by addition of a solution (0.1 mL) of 4 M HCl in ethyl acetate
  9. stirringthe mixture was stirred at room temperature for 3.5 h
  10. customThe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-c11da105693044f4b75eabd9408079ea
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…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート