Chloroacetyl chloride → N'-(2,6-dichloro-4-trifluoromethylphenyl)-chloroacetohydrazide

HRID 1167990

反応式

HRID 1167990 の反応式
[Cl:1][CH2:2][C:3](Cl)=[O:4].[Cl:6][C:7]1[CH:12]=[C:11]([C:13]([F:16])([F:15])[F:14])[CH:10]=[C:9]([Cl:17])[C:8]=1[NH:18][NH2:19].[OH-].[Na+]>ClCCl>[Cl:6][C:7]1[CH:12]=[C:11]([C:13]([F:15])([F:14])[F:16])[CH:10]=[C:9]([Cl:17])[C:8]=1[NH:18][NH:19][C:3](=[O:4])[CH2:2][Cl:1]

参加物

5

反応物 3

HCID 6577Chloroacetyl chlorideHCID 14798Sodium HydroxideHCID 688223[2,6-Dichloro-4-(trifluoromethyl)phenyl]hydrazine

生成物 1

HCID 22015908N'-(2,6-dichloro-4-trifluoromethylphenyl)-chloroacetohydrazide収率 91%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒3 回

反応条件

温度
20 °C

実験手順

A solution of chloroacetyl chloride (2.3 ml, 1.08 equivalents) in anhydrous dichloromethane (30 ml) was added during 30 minutes to a stirred solution of 2,6-dichloro-4-trifluoromethylphenylhydrazine (6.1 g, 24.89 mmol) in anhydrous dichloromethane (60 ml) maintaining between 5 and 12° C. under an argon atmosphere. The mixture was then stirred for 5-12 hours at 20° C. A solution of sodium hydroxide (11.2 ml of 10%) and dichloromethane were added and the organic phase washed (water), dried (magnesium sulphate) and evaporated to give the title compound (7.25 g) as a white solid, NMR 4.05(s,2H), 6.77(s,1H), 7.47(s,2H), 8.6(s,1H). The yield was 91%.

後処理

  1. temperaturemaintaining between 5 and 12° C. under an argon atmosphere
  2. washthe organic phase washed (water)
  3. dry with materialdried (magnesium sulphate)
  4. customevaporated

出典と根拠

ORDレコード
ord-652551da83094411bc3efd8518de0567
出典データセット
uspto-grants-2003_09
特許番号
US06620944B1

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