Sulfamide → HCID 178418935、化合物

HRID 894309

反応式

HRID 894309 の反応式
[NH:1]([C:5]1[S:6][CH:7]=[C:8]([CH2:10][S:11][CH2:12][CH2:13][C:14](=[NH:17])OC)[N:9]=1)[C:2]([NH2:4])=[NH:3].[S:18]([NH2:22])([NH2:21])(=[O:20])=[O:19]>CO>[S:18]([NH:22][C:14](=[NH:17])[CH2:13][CH2:12][S:11][CH2:10][C:8]1[N:9]=[C:5]([NH:1][C:2]([NH2:4])=[NH:3])[S:6][CH:7]=1)(=[O:20])(=[O:19])[NH2:21]

参加物

4

反応物 2

HCID 82267SulfamideHCID 12881442Methyl 3-[({2-[(diaminomethylidene)amino]-1,3-thiazol-4-yl}methyl)sulfanyl]propanimidate

生成物 1

HCID 178418935HCID 178418935、化合物収率 64.6%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

In 30 ml of methanol was dissolved 4.09 g of methyl 3-[(2-guanidinothiazol-4-yl)methylthio]propionimidate and then 15 ml of a methanol solution of 2.88 g of sulfamide was added to the solution under refluxing. After refluxing for about 3 hours, the solvent was distilled off under reduced pressure and the residue was purified by a silica gel column chromatography using a mixture of chloroform and methanol (20:1→10:1) as the developing solvent to provide 3,26 g of N-sulfamoyl-3-[(2-guanidinothiazol-4-yl)methylthio]propionamidine. The product shows the following physical chemical properties:

後処理

  1. temperatureunder refluxing
  2. temperatureAfter refluxing for about 3 hours
  3. distillationthe solvent was distilled off under reduced pressure
  4. customthe residue was purified by a silica gel column chromatography
  5. additiona mixture of chloroform and methanol (20:1→10:1) as the developing solvent

出典と根拠

ORDレコード
ord-7def2468710f4341bfe8365e21667ccb
出典データセット
uspto-grants-1981_08
特許番号
US04283408

関連ノート

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