Carbon Tetrachloride → 1,1,1,3,3,3-Hexachloropropane

HRID 1383890

반응식

HRID 1383890 반응식
[ClH:1].C(N(CC)CC)C.C(#N)CCCCC#N.[C:17]([Cl:21])([Cl:20])([Cl:19])Cl.[C:22]([Cl:25])([Cl:24])=[CH2:23]>[Ni]>[Cl:24][C:22]([Cl:1])([Cl:25])[CH2:23][C:17]([Cl:21])([Cl:20])[Cl:19]

참가 물질

6

반응물 4

HCID 5943Carbon TetrachlorideHCID 6366Vinylidene chlorideHCID 8128AdiponitrileHCID 11130Triethylamine hydrochloride

생성물 1

HCID 192151,1,1,3,3,3-Hexachloropropane

시약·촉매·용매 1

HCID 935Nickel촉매

반응 조건

온도
120 °C

실험 절차

A 400 mL Hastelloy™ C nickel alloy shaker tube was charged with anhydrous cuprous chloride (1.39 g, 0.014 mole), triethylamine hydrochloride (1.93 g, 0.014 mole), adiponitrile (52.0 g, 0.481 mole), carbon tetrachloride (151.0 g, 0.982 mole), and vinylidene chloride (47.5 g, 0.490 mole). The tube was sealed, cooled in a dry ice bath, evacuated, and purged with nitrogen several times. The tube was placed in a heating jacket and agitation begun. The tube was heated to 120° C. over the course of 1.3 hours and then held at 119-122° C. for one hour; during this time the pressure rose to a maximum of 83 psig (674 kPa) and then dropped to 41 psig (384 kPa) at the end of the heating period. The tube was then cooled to ambient temperature.

후처리

  1. customThe tube was sealed
  2. temperaturecooled in a dry ice bath
  3. customevacuated
  4. custompurged with nitrogen several times
  5. additiondropped to 41 psig (384 kPa) at the end of the heating period
  6. temperatureThe tube was then cooled to ambient temperature

출처 및 근거

ORD 기록
ord-9875189777e442668b5f2558a342c96e
출처 데이터셋
uspto-grants-2001_07
특허 번호
US06255544B1

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