2-(Chloromethyl)-3,4-dimethoxypyridin-1-ium chloride → HCID 178493203, 화합물

HRID 845518노트

반응식

HRID 845518 반응식
[Cl-].Cl[CH2:3][C:4]1[C:9]([O:10][CH3:11])=[C:8]([O:12][CH3:13])[CH:7]=[CH:6][NH+:5]=1.[SH:14][C:15]1[NH:19][C:18]2[CH:20]=[CH:21][C:22]([O:24][C:25]([F:30])([F:29])[CH:26]([F:28])[F:27])=[CH:23][C:17]=2[N:16]=1>C(O)C.O.[OH-].[Na+]>[CH3:11][O:10][C:9]1[C:4]([CH2:3][S:14][C:15]2[NH:19][C:18]3[CH:20]=[CH:21][C:22]([O:24][C:25]([F:30])([F:29])[CH:26]([F:28])[F:27])=[CH:23][C:17]=3[N:16]=2)=[N:5][CH:6]=[CH:7][C:8]=1[O:12][CH3:13]

참가 물질

6

반응물 2

HCID 248204092-(Chloromethyl)-3,4-dimethoxypyridin-1-ium chlorideHCID 178506049HCID 178506049, 화합물

생성물 1

HCID 178493203HCID 178493203, 화합물

시약·촉매·용매 3

HCID 702Ethanol용매HCID 962Water용매2회HCID 14798Sodium Hydroxide용매

반응 조건

온도
20 °C

실험 절차

0.38 g (1.7 mmol) of 2-chloromethyl-3,4-dimethoxypyridinium chloride is added to a solution of 0.46 g (1.7 mmol) of 2-mercapto-5-(1,1,2,2-tetra fluoroethoxy)-1H-benzimidazole in 10 ml of ethanol, 10 ml of water and 1.8 ml of 2N sodium hydroxide solution; after the mixture has been stirred at 20° C. for one hour, a further 10 ml of water are added dropwise. The mixture is then stirred at 20° C. for a further four hours. The solid which has precipitated out is filtered off, washed with 0.01N sodium hydroxide solution and then with water until neutral and dried to constant weight. 0.63 g (90% of theory) of the title compound is obtained as a colorless crystalline powder of m.p. 98°-102° C.

후처리

  1. stirringThe mixture is then stirred at 20° C. for a further four hours
  2. customThe solid which has precipitated out
  3. filtrationis filtered off
  4. washwashed with 0.01N sodium hydroxide solution
  5. dry with materialwith water until neutral and dried to constant weight

출처 및 근거

ORD 기록
ord-b61163aa447a43309b6dc8594a674096
출처 데이터셋
uspto-grants-1988_07
특허 번호
US04758579

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