Water → HCID 178501896、化合物

HRID 230736

反応式

HRID 230736 の反応式
S(OS([O-])=O)([O-])=O.[Na+].[Na+].[Cl:10][C:11]1[S:12][C:13]([CH:16]=O)=[CH:14][CH:15]=1.[NH2:18][C:19]1[CH:20]=[C:21]([S:26]([CH2:29][C:30]([O:32][CH3:33])=[O:31])(=[O:28])=[O:27])[CH:22]=[CH:23][C:24]=1[NH2:25].O>CN1CCCC1=O>[Cl:10][C:11]1[S:12][C:13]([C:16]2[NH:25][C:24]3[CH:23]=[CH:22][C:21]([S:26]([CH2:29][C:30]([O:32][CH3:33])=[O:31])(=[O:28])=[O:27])=[CH:20][C:19]=3[N:18]=2)=[CH:14][CH:15]=1

参加物

6

反応物 4

HCID 962WaterHCID 24346Disodium disulfiteHCID 817002-Thiophenecarboxaldehyde, 5-chloro-HCID 57763314Methyl (3,4-diaminobenzenesulfonyl)acetate

生成物 1

HCID 178501896HCID 178501896、化合物

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
110 °C

実験手順

14.4 747 mg (3.93 mmol) of sodium disulfite are added to a solution of 1.15 g (7.86 mmol) of 2-chlorothiophene-5-carbaldehyde and 1.92 g (7.86 mmol) of methyl (3,4-diaminobenzenesulfonyl)acetate in 25 ml of 1-methylpyrrolidone, and the mixture is stirred at 110° C. for 18 hours. Water is added to the reaction mixture, which is extracted with dichloromethane. The organic phase is dried over sodium sulfate and evaporated. The residue is stirred with water, and the resultant precipitate is filtered off, giving methyl [2-(5-chlorothiophen-2-yl)-1H-benzimidazole-5-sulfonyl]-acetate as a brown solid; ESI 371.

後処理

  1. extractionis extracted with dichloromethane
  2. dry with materialThe organic phase is dried over sodium sulfate
  3. customevaporated
  4. stirringThe residue is stirred with water
  5. filtrationthe resultant precipitate is filtered off

出典と根拠

ORDレコード
ord-f5de34153b9b43da8657d33176101420
出典データセット
uspto-grants-2009_07
特許番号
US07566789B2

関連ノート

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