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

HRID 1385999ノート

反応式

HRID 1385999 の反応式
[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

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 129286411-(4-Chlorobutoxy)-3-(trifluoromethyl)-benzeneHCID 178514135HCID 178514135、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-bab109de64834d62a2577824483e6111
出典データセット
uspto-grants-2001_07
特許番号
US06265407B1

反応ノート

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