p-Bromobenzenesulfonyl chloride → HCID 69206070、化合物

HRID 901960ノート

反応式

HRID 901960 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([S:8](Cl)(=[O:10])=[O:9])=[CH:4][CH:3]=1.[CH3:12][NH:13][CH2:14][C:15]1[S:16][CH:17]=[C:18]([C:20]([O:22][CH2:23][CH3:24])=[O:21])[N:19]=1.C(N(CC)CC)C>ClCCl.C(OCC)(=O)C>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([N:13]([CH2:14][C:15]2[S:16][CH:17]=[C:18]([C:20]([O:22][CH2:23][CH3:24])=[O:21])[N:19]=2)[CH3:12])(=[O:10])=[O:9])=[CH:4][CH:3]=1

参加物

6

反応物 3

HCID 7396p-Bromobenzenesulfonyl chlorideHCID 8471TriethylamineHCID 45117596Ethyl 2-(methylaminomethyl)thiazole-4-carboxylate

生成物 1

HCID 69206070HCID 69206070、化合物収率 67%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

4-Bromobenzenesulfonyl chloride (2.1 g, 8.2 mmol) was added to a solution of ethyl 2-(methylaminomethyl)thiazole-4-carboxylate (1.5 g, 7.5 mmol) and triethylamine (2.1 ml, 1.5 g, 15 mmol) in dichloromethane (30 ml) and the mixture was stirred for 18 h. The mixture was diluted with ethyl acetate and washed with 1N potassium hydrogen sulphate, water and brine, dried and reduced. Chromatography (35% EtOAc/65% hexanes) afforded ethyl 2-(N-(4-bromobenzenesulphonyl)-N-methylaminomethyl)thiazole-4-carboxylate (2.1 g, 67%) as a white solid.

後処理

  1. washwashed with 1N potassium hydrogen sulphate, water and brine
  2. customdried

出典と根拠

ORDレコード
ord-757e8e0983414520884302abbbbb2205
出典データセット
uspto-grants-2008_04
特許番号
US07365065B2

反応ノート

読み込み中…