Water → 3,4-Dichloro-1-methyl-5-(propylsulfanyl)-1H-pyrazole

HRID 1632729ノート

反応式

HRID 1632729 の反応式
[CH2:1]([SH:4])[CH2:2][CH3:3].[OH-].[K+].[CH3:7][N:8]1[C:12](Cl)=[C:11]([Cl:14])[C:10]([Cl:15])=[N:9]1.O>CS(C)=O>[CH3:7][N:8]1[C:12]([S:4][CH2:1][CH2:2][CH3:3])=[C:11]([Cl:14])[C:10]([Cl:15])=[N:9]1

参加物

6

反応物 4

HCID 962WaterHCID 7848Propyl mercaptanHCID 14797Potassium HydroxideHCID 14751841H-Pyrazole, 3,4,5-trichloro-1-methyl-

生成物 1

HCID 133743743,4-Dichloro-1-methyl-5-(propylsulfanyl)-1H-pyrazole

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

反応条件

温度
120 °C

実験手順

A stirred mixture of 4.9 g (0.064 moles) propanthiol and 3 g (0.054 moles) potassium hydroxide in 50 ml dimethylsulfoxide was heated (at about 120° C.) for thirty minutes. Then 10 g (0.054 moles) 1-methyl-3,4,5-trichloropyrazole was added in one portion. Heating (at about 120° C.) of the stirred reaction mixture was continued for about 6 hours. The reaction mixture was allowed to cool. The reaction mixture was added to water (about 50 ml); the resulting mixture was extracted with ether. The etheral phase was separated, washed with water twice, and dried over magnesium sulfate. The solvent was then stripped. The product was distilled out at 124° C. under high vacuum and heat.

後処理

  1. temperatureHeating
  2. custom(at about 120° C.) of the stirred reaction mixture
  3. temperatureto cool
  4. extractionthe resulting mixture was extracted with ether
  5. customThe etheral phase was separated
  6. washwashed with water twice
  7. dry with materialdried over magnesium sulfate
  8. distillationThe product was distilled out at 124° C. under high vacuum
  9. temperatureheat

出典と根拠

ORDレコード
ord-11451eb847714e94a1bc5d892792080c
出典データセット
uspto-grants-1984_10
特許番号
US04477462

反応ノート

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