Water → HCID 178501896, 화합물

HRID 230736

반응식

HRID 230736 반응식
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

참가 물질

6

반응물 4

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

생성물 1

HCID 178501896HCID 178501896, 화합물

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

반응 조건

온도
110 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f5de34153b9b43da8657d33176101420
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07566789B2

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