Sodium Hydroxide → HCID 18471605、化合物

HRID 381219

反応式

HRID 381219 の反応式
[C:1]([C:3]1[CH:11]=[CH:10][C:6]([C:7](Cl)=[O:8])=[CH:5][CH:4]=1)#[N:2].[Cl:12][C:13]1[CH:18]=[C:17]([C:19]([F:22])([F:21])[F:20])[CH:16]=[C:15]([Cl:23])[C:14]=1[NH:24][NH2:25].[OH-].[Na+]>C(Cl)Cl>[Cl:12][C:13]1[CH:18]=[C:17]([C:19]([F:21])([F:20])[F:22])[CH:16]=[C:15]([Cl:23])[C:14]=1[NH:24][NH:25][C:7](=[O:8])[C:6]1[CH:10]=[CH:11][C:3]([C:1]#[N:2])=[CH:4][CH:5]=1

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 801724-Cyanobenzoyl chlorideHCID 688223[2,6-Dichloro-4-(trifluoromethyl)phenyl]hydrazine

生成物 1

HCID 18471605HCID 18471605、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒3 回

実験手順

A solution of 14.2 g of 4-cyanobenzoyl chloride in 100 ml of methylene chloride is added dropwise with stirring at from 10 to 15° in the course of approximately 30 minutes to 20 g of 2,6-dichloro-4-trifluoromethylphenylhydrazine in 250 ml of dichloromethane, and the mixture is stirred for a further 16 hours. 36 ml of aqueous sodium hydroxide solution (10%) is then run in with vigorous stirring. 100 ml of methylene chloride are added, the organic phase is washed three times using in each case 100 ml of water and dried over sodium sulfate, and the solvent is removed on a rotary evaporator. After the residue has been recrystallized from toluene, the title product of melting point 185-186° is obtained (compound no. 1.6).

後処理

  1. washthe organic phase is washed three times
  2. dry with materialdried over sodium sulfate
  3. customthe solvent is removed on a rotary evaporator
  4. customAfter the residue has been recrystallized from toluene

出典と根拠

ORDレコード
ord-f6a9b79096a94eb8af4cf78b3abf1bad
出典データセット
uspto-grants-2001_10
特許番号
US06306798B1

関連ノート

読み込み中…