Dichloromethane → 1.1,3-Trichloropentane-1-phosponic dichloride

HRID 1438902

반응식

HRID 1438902 반응식
[CH3:1][CH2:2][CH:3]=[CH2:4].[Cl:5][C:6]([Cl:12])(Cl)[P:7]([Cl:10])([Cl:9])=[O:8].C(Cl)[Cl:14]>C1C(C(OOC(C)(C)C)=O)=CC=CC=1>[Cl:5][C:6]([Cl:12])([P:7]([Cl:10])([Cl:9])=[O:8])[CH2:4][CH:3]([Cl:14])[CH2:2][CH3:1]

참가 물질

5

반응물 3

HCID 6344DichloromethaneHCID 78441-ButeneHCID 277422(Trichloromethyl)phosphonic dichloride

생성물 1

HCID 213996821.1,3-Trichloropentane-1-phosponic dichloride

시약·촉매·용매 1

HCID 11966tert-Butyl peroxybenzoate촉매

실험 절차

5.6 g (0.1 mole)butene-1, 71 g (0.3 mole) trichloromethane phosphonic dichloride and 0.5 g tert. butyl perbenzoate were heated in 100 ml methylene chloride in a closed ampoule and in the absence of air, during 10 hours at 120°. After cooling, the ampoule was opened and its contents distilled. Unconverted trichloromethane phosphonic dichloride sublimed between 70° and 125° at 25 mm pressure. The continued distillation yielded 10.3 g 1.1,3-trichloropentane-1-phosponic dichloride, bp/0.05: 64°-66°. Found Cl: 61.3%. Calc. for C5H8Cl5OP: 61.0%.

후처리

  1. temperatureAfter cooling
  2. distillationits contents distilled
  3. customUnconverted trichloromethane phosphonic dichloride sublimed between 70° and 125°
  4. distillationThe continued distillation

출처 및 근거

ORD 기록
ord-03a4e42918c740d6a2b5f4990a17870d
출처 데이터셋
uspto-grants-1977_11
특허 번호
US04057579

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