1,8-Diazabicyclo(5.4.0)undec-7-ene → 4,5-Dihydro-2-(2-sulfamoylphenylmethylthio)thiazole

HRID 746125

反応式

HRID 746125 の反応式
N12CCCN=C1CCCCC2.[SH:12][C:13]1[S:14][CH2:15][CH2:16][N:17]=1.Cl[CH2:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=1[S:26]([NH2:29])(=[O:28])=[O:27]>C(#N)C.O>[S:26]([C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=1[CH2:19][S:12][C:13]1[S:14][CH2:15][CH2:16][N:17]=1)(=[O:27])(=[O:28])[NH2:29]

参加物

6

反応物 3

HCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 133646272-(Chloromethyl)benzenesulfonamideHCID 178527880HCID 178527880、化合物

生成物 1

HCID 200417444,5-Dihydro-2-(2-sulfamoylphenylmethylthio)thiazole収率 82.4%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6342Acetonitrile溶媒

実験手順

With cooling, 7.9 g of 97%, 1,8-diazabicyclo[5.4.0]undec-7-ene are added to a suspension of 6.2 g of 97% 4,5-dihydro-2-mercaptothiazole in 50 ml of acetonitrile. To the yellow solution so obtained are added 10.3 g of 2-chloromethylbenzenesulfonamide and the reaction mixture is stirred for 1 hour at 20°-25° C. The reaction solution is then diluted with about 1 liter of water. The precipitate is isolated by filtration and dried, affording 11.9 g (76% of theory) of 4,5-dihydro-2-(2-sulfamoylphenylmethylthio)thiazole of m.p. 123°-125° C.

後処理

  1. temperatureWith cooling
  2. customTo the yellow solution so obtained
  3. customThe precipitate is isolated by filtration
  4. customdried

出典と根拠

ORDレコード
ord-e88c4d94745a4fe5a5b6a107403b11c0
出典データセット
uspto-grants-1986_07
特許番号
US04602936

関連ノート

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