3-Fluorobenzoyl chloride → HCID 15733509、化合物

HRID 341862ノート

反応式

HRID 341862 の反応式
[CH3:1][N:2]([C:4]([NH:6][CH3:7])=[S:5])[NH2:3].[F:8][C:9]1[CH:10]=[C:11]([CH:15]=[CH:16][CH:17]=1)[C:12](Cl)=[O:13]>N1C=CC=CC=1>[CH3:1][N:2]([C:4]([NH:6][CH3:7])=[S:5])[NH:3][C:12](=[O:13])[C:11]1[CH:15]=[CH:16][CH:17]=[C:9]([F:8])[CH:10]=1

参加物

4

反応物 2

HCID 743763-Fluorobenzoyl chlorideHCID 30341872,4-Dimethylthiosemicarbazide

生成物 1

HCID 15733509HCID 15733509、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To a stirred, room temperature, solution of 2,4-dimethylthiosemicarbazide (5.96 g, 50.0 mmol) and dry pyridine (100 mL) was added dropwise 3-fluorobenzoyl chloride (7.93 g, 50.0 mmol). After stirring overnight, the reaction mixture was evaporated at reduced pressure. The concentrate was slurried with water and that which did not dissolve was collected by filtration. Crystallization of this material from ethanol afforded the desired product as colorless needles, mp 202°-205° C.

後処理

  1. customthe reaction mixture was evaporated at reduced pressure
  2. dissolutiondid not dissolve
  3. filtrationwas collected by filtration
  4. customCrystallization of this material from ethanol

出典と根拠

ORDレコード
ord-5115182a487c49d49645869cd541a055
出典データセット
uspto-grants-1999_01
特許番号
US05856350

反応ノート

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