1,3-Butadiene → 1,1,5-Trichloro-pent-3-ene-1-phosphonic dichloride

HRID 1438900

반응식

HRID 1438900 반응식
[Cl:1][C:2]([Cl:8])(Cl)[P:3]([Cl:6])([Cl:5])=[O:4].[CH2:9]=[CH:10][CH:11]=[CH2:12].[Cl-:13].C([NH+](CC)CC)C>C(Cl)Cl>[Cl:1][C:2]([Cl:8])([P:3]([Cl:6])([Cl:5])=[O:4])[CH2:9][CH:10]=[CH:11][CH2:12][Cl:13]

참가 물질

5

반응물 3

HCID 78451,3-ButadieneHCID 277422(Trichloromethyl)phosphonic dichlorideHCID 12698378Triethylazanium chloride

생성물 1

HCID 541714891,1,5-Trichloro-pent-3-ene-1-phosphonic dichloride

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

11.8 g (0.05 mole) trichloromethane phosphonic dichloride was dissolved in 10 ml dry methylene chloride, cooled, and a cold solution of 4 g butadiene in 10 ml methylene chloride, which also contained 134 mg (1 mmole) anhydrous cupric chloride and 206 mg (1.5 mmole) triethylammonium chloride, was added. The resulting homogeneous solution was heated in the absence of air, in a sealed ampoule, at 100° for 8 hours. After cooling, the reaction product was freed from solvent, and fractionated through a short Vigreux column. 9.6 g pure 1:1 adduct, 1,1,5-trichloro-pent-3-ene-1-phosphonic dichloride was obtained, bp/0.05: 92° -93°. Found: Cl: 61.3%, Calc. for C5H6Cl5OP: 61.0%.

후처리

  1. temperaturecooled
  2. temperatureThe resulting homogeneous solution was heated in the absence of air
  3. temperatureAfter cooling

출처 및 근거

ORD 기록
ord-e853973cd3c74b0e94fcf182e4c51b54
출처 데이터셋
uspto-grants-1977_11
특허 번호
US04057578

연결된 노트

불러오는 중…