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

HRID 1167989

반응식

HRID 1167989 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
70 °C

실험 절차

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%.

후처리

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

출처 및 근거

ORD 기록
ord-af87d60130954e7ba890461923cb8d72
출처 데이터셋
uspto-grants-2003_09
특허 번호
US06620944B1

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