Phosphorus oxychloride → N'-(2,6-dichloro-4-trifluoromethylphenyl)-chloroacetohydrazonoyl chloride

HRID 8420

反応式

HRID 8420 の反応式
P(Cl)(Cl)([Cl:3])=O.[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][NH:19][C:20](=O)[CH2:21][Cl:22]>C1(C)C=CC=CC=1>[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][N:19]=[C:20]([Cl:3])[CH2:21][Cl:22]

参加物

4

反応物 2

HCID 24813Phosphorus oxychlorideHCID 22015908N'-(2,6-dichloro-4-trifluoromethylphenyl)-chloroacetohydrazide

生成物 1

HCID 86591113N'-(2,6-dichloro-4-trifluoromethylphenyl)-chloroacetohydrazonoyl chloride収率 90%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
70 °C

実験手順

Phosphoryl chloride (500 microlitres, 1.7 equivalents) was added in one portion to a stirred solution of N′-(2,6-dichloro-4-trifluoromethylphenyl)-chloroacetohydrazide (1.0 g, 3.11 mmol) in toluene (20 ml) and heated at 70° C. under an argon atmosphere for 20 hours. The cooled mixture was evaporated and the residue extracted with cyclohexane. The extracts were combined and evaporated to give the title compound (0.971 g) as an orange oil, NMR 4.4 (s, 2H), 7.55 (s, 2H), 7.7 (s, 1H). The yield was 90%.

後処理

  1. customThe cooled mixture was evaporated
  2. extractionthe residue extracted with cyclohexane
  3. customevaporated

出典と根拠

ORDレコード
ord-9a91687510384f2a99c8906dc00af77d
出典データセット
uspto-grants-2006_08
特許番号
US07087786B2

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