Sodium hydride → 6-[[4-[3-(Trifluoromethyl)-phenoxy]butyl]thio]-3-pyridazinecarbothioamide

HRID 1385999노트

반응식

HRID 1385999 반응식
[SH:1][C:2]1[N:7]=[N:6][C:5]([C:8](=[S:10])[NH2:9])=[CH:4][CH:3]=1.[H-].[Na+].Cl[CH2:14][CH2:15][CH2:16][CH2:17][O:18][C:19]1[CH:24]=[CH:23][CH:22]=[C:21]([C:25]([F:28])([F:27])[F:26])[CH:20]=1>CN(C=O)C>[F:26][C:25]([F:27])([F:28])[C:21]1[CH:20]=[C:19]([CH:24]=[CH:23][CH:22]=1)[O:18][CH2:17][CH2:16][CH2:15][CH2:14][S:1][C:2]1[N:7]=[N:6][C:5]([C:8](=[S:10])[NH2:9])=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 129286411-(4-Chlorobutoxy)-3-(trifluoromethyl)-benzeneHCID 178514135HCID 178514135, 화합물

생성물 1

HCID 181766426-[[4-[3-(Trifluoromethyl)-phenoxy]butyl]thio]-3-pyridazinecarbothioamide

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

A mixture of intermediate 11 (0.017 mol) in DMF (80 ml) was stirred at room temperature. Sodium hydride (50%, 0.02 mol) was added portionwise. The mixture was stirred for 30 minutes. A mixture of 1-(4-chlorobutoxy)-3-(trifluoromethyl)-benzene (0.02 mol) in DMF (20 ml) was added dropwise. The mixture was stirred at room temperature overnight. The solvent was evaporated. The residue was stiffed in DIPE (100 ml), filtered off and dried, yielding 3.lg (47%) of 6-[[4-[3-(trifluoromethyl)-phenoxy]butyl]thio]-3-pyridazinecarbothioamide (intermediate 12).

후처리

  1. stirringThe mixture was stirred for 30 minutes
  2. additionwas added dropwise
  3. stirringThe mixture was stirred at room temperature overnight
  4. customThe solvent was evaporated
  5. filtrationfiltered off
  6. customdried

출처 및 근거

ORD 기록
ord-bab109de64834d62a2577824483e6111
출처 데이터셋
uspto-grants-2001_07
특허 번호
US06265407B1

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