Water → HCID 178493767, 화합물

HRID 845515노트

반응식

HRID 845515 반응식
[SH:1][C:2]1[NH:6][C:5]2[CH:7]=[CH:8][C:9]([O:11][CH2:12][C:13]([F:16])([F:15])[F:14])=[CH:10][C:4]=2[N:3]=1.[Cl-].Cl[CH2:19][C:20]1[CH:25]=[C:24]([O:26][CH3:27])[C:23]([O:28][CH3:29])=[CH:22][NH+:21]=1.O>C(O)C.[OH-].[Na+]>[CH3:27][O:26][C:24]1[C:23]([O:28][CH3:29])=[CH:22][N:21]=[C:20]([CH2:19][S:1][C:2]2[NH:6][C:5]3[CH:7]=[CH:8][C:9]([O:11][CH2:12][C:13]([F:16])([F:14])[F:15])=[CH:10][C:4]=3[N:3]=2)[CH:25]=1

참가 물질

6

반응물 3

HCID 962WaterHCID 201313622-Chloromethyl-4,5-dimethoxypyridinium chlorideHCID 178506345HCID 178506345, 화합물

생성물 1

HCID 178493767HCID 178493767, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 14798Sodium Hydroxide용매

실험 절차

1.0 g of 2-mercapto-5-(2,2,2-trifluoroethoxy)-1H-benzimidazole is dissolved in 15 ml of ethanol and 8.5 ml of 1N sodium hydroxide solution, 0.90 g of 2-chloromethyl-4,5-dimethoxypyridinium chloride are added and the mixture is stirred for 20 hours. After addition of 30 ml of water, the mixture is extracted three times with 30 ml of methylene chloride each time, the methylene chloride phase is washed once with 5 ml of 0.1N sodium hydroxide solution, the combined organic phases are dried over magnesium sulfate and, after the drying agent has been filtered off, the filtrate is completely concentrated. 1.51 g (94% of theory) of the title compound are obtained as an amorphous solid residue of m.p. 55°-57° C.

후처리

  1. extractionthe mixture is extracted three times with 30 ml of methylene chloride each time
  2. washthe methylene chloride phase is washed once with 5 ml of 0.1N sodium hydroxide solution
  3. dry with materialthe combined organic phases are dried over magnesium sulfate
  4. filtrationafter the drying agent has been filtered off
  5. concentrationthe filtrate is completely concentrated

출처 및 근거

ORD 기록
ord-6b38d607ed584f6d874e70a98ec97057
출처 데이터셋
uspto-grants-1988_07
특허 번호
US04758579

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