Dicyclohexylamine → 2-(3,3-Dicyclohexylureido)-4-methylthiazole-5-carboxylic acid (2-hydroxyethyl)amide

HRID 731409

反応式

HRID 731409 の反応式
[OH:1][CH2:2][CH2:3][NH:4][C:5]([C:7]1(N)NC(C)=C[S:8]1)=[O:6].CC(O[Si](C)(C)C)=N[Si](C)(C)C.C1N=CN([C:31]([N:33]2[CH:37]=[N:36][CH:35]=[CH:34]2)=[O:32])C=1.[CH:38]1([NH:44][CH:45]2[CH2:50][CH2:49][CH2:48][CH2:47][CH2:46]2)[CH2:43][CH2:42][CH2:41][CH2:40][CH2:39]1>ClCCl.CN(C1C=CN=CC=1)C>[OH:1][CH2:2][CH2:3][NH:4][C:5]([C:7]1[S:8][C:37]([NH:33][C:31]([N:44]([CH:38]2[CH2:39][CH2:40][CH2:41][CH2:42][CH2:43]2)[CH:45]2[CH2:46][CH2:47][CH2:48][CH2:49][CH2:50]2)=[O:32])=[N:36][C:35]=1[CH3:34])=[O:6]

参加物

7

反応物 4

HCID 7582DicyclohexylamineHCID 25248trimethylsilyl N-trimethylsilylethanimidateHCID 682631,1'-CarbonyldiimidazoleHCID 866301872-Amino-4-methyl-thiazole-carboxylic acid (2-hydroxyethyl)-amide

生成物 1

HCID 576882882-(3,3-Dicyclohexylureido)-4-methylthiazole-5-carboxylic acid (2-hydroxyethyl)amide

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒

実験手順

To a mixture of 2-amino-4-methyl-thiazole-carboxylic acid (2-hydroxyethyl)-amide (0.2 g) in dichloromethane was added N,O-bis-(trimethylsilyl)-acetamide (0.2 g) and the mixture stirred for 12 h. CDI (0.16 g) and DMAP (6 mg) was then added and the mixture stirred for 12 h before addition of dicyclohexylamine (0.18 g). After stirring overnight waster was added and the aqueous phase extracted with dichloromethane, concentrated and purified by chromatography to give the title compound.

後処理

  1. stirringAfter stirring overnight waster
  2. additionwas added
  3. extractionthe aqueous phase extracted with dichloromethane
  4. concentrationconcentrated
  5. custompurified by chromatography

出典と根拠

ORDレコード
ord-2d4de976a669412394bdef82b98537b3
出典データセット
uspto-grants-2009_09
特許番号
US07582769B2

関連ノート

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