Diethyl Ether → (s)-2-(4-Nitrophenyl)-1-(2-phenylthiazol-4-yl)ethanamine hydrobromide salt

HRID 424892

反応式

HRID 424892 の反応式
C(OC(=O)[NH:7][CH:8]([CH2:13][C:14]1[CH:19]=[CH:18][C:17]([N+:20]([O-:22])=[O:21])=[CH:16][CH:15]=1)[C:9](=O)[CH2:10][Br:11])(C)(C)C.[C:24](=[S:32])([NH2:31])[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1.C(OCC)C>CC#N>[BrH:11].[N+:20]([C:17]1[CH:16]=[CH:15][C:14]([CH2:13][C@@H:8]([C:9]2[N:31]=[C:24]([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=3)[S:32][CH:10]=2)[NH2:7])=[CH:19][CH:18]=1)([O-:22])=[O:21]

参加物

5

反応物 3

HCID 3283Diethyl EtherHCID 683563ThiobenzamideHCID 76068232[3-Bromo-1-(4-nitro-benzyl)-2-oxo-propyl]-carbamic acid tert-butyl ester

生成物 1

HCID 66704795(s)-2-(4-Nitrophenyl)-1-(2-phenylthiazol-4-yl)ethanamine hydrobromide salt収率 63%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A mixture of [3-bromo-1-(4-nitro-benzyl)-2-oxo-propyl]-carbamic acid tert-butyl ester, 37, (1.62 g, 4.17 mmol) and benzothioamide (0.630 g, 4.59 mmol), in CH3CN (5 mL) is refluxed for 24 hours. The reaction mixture is cooled to room temperature and diethyl ether (50 mL) is added to the solution and the precipitate that forms is collected by filtration. The solid is dried under vacuum to afford 1.059 g (63%) of the desired product. ESI+ MS 326 (M+1).

後処理

  1. filtrationthe precipitate that forms is collected by filtration
  2. customThe solid is dried under vacuum

出典と根拠

ORDレコード
ord-38b08f4bb9f74240907d46880e2bb8b8
出典データセット
uspto-grants-2012_01
特許番号
US08106078B2

関連ノート

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