Water → HCID 178470643、化合物

HRID 230731

反応式

HRID 230731 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]([CH2:26][C:27]([O:29][CH2:30][CH3:31])=[O:28])[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]([CH2:26][C:27]([O:29][CH2:30][CH3:31])=[O:28])=[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 12986345Ethyl 2-(3,4-diaminophenyl)acetate

生成物 1

HCID 178470643HCID 178470643、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

3.1 3.89 g (20.5 mmol) of sodium disulfite are added to a solution of 3.00 g (20.5 mmol) of 2-chlorothiophene-5-carbaldehyde and 3.98 g (20.5 mmol) of ethyl 3,4-diaminophenylacetate in 30 ml of 1-methyl-pyrrolidone, 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 using sodium sulfate and evaporated, giving ethyl [2-(5-chlorothiophen-2-yl)-1H-benzimidazol-5-yl]acetate as a brown oil (ESI 321), which is employed without further purification for the next reaction.

後処理

  1. extractionis extracted with dichloromethane
  2. customThe organic phase is dried
  3. customevaporated

出典と根拠

ORDレコード
ord-007244662b1a4f669932ccf3d84cc4e2
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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