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

HRID 1438900

反応式

HRID 1438900 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

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%.

後処理

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

出典と根拠

ORDレコード
ord-e853973cd3c74b0e94fcf182e4c51b54
出典データセット
uspto-grants-1977_11
特許番号
US04057578

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