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

HRID 1383890

反応式

HRID 1383890 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 935Nickel触媒

反応条件

温度
120 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9875189777e442668b5f2558a342c96e
出典データセット
uspto-grants-2001_07
特許番号
US06255544B1

関連ノート

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