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

HRID 896798

반응식

HRID 896798 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 microliters, 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-2179bc0357b14a7a9705aade40505697
출처 데이터셋
uspto-grants-2005_07
특허 번호
US06919462B2

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