2,2-dimethylhexanedinitrile → HCID 11815890、化合物

HRID 1699123ノート

反応式

HRID 1699123 の反応式
CC(C)([O-:4])C.[K+].[CH3:7][C:8]([CH3:16])([CH2:11][CH2:12][CH2:13][C:14]#[N:15])[C:9]#N>C1(C)C=CC=CC=1>[C:14]([CH:13]1[C:7](=[O:4])[C:8]([CH3:16])([CH3:9])[CH2:11][CH2:12]1)#[N:15]

参加物

4

反応物 2

HCID 2642192,2-dimethylhexanedinitrileHCID 23665647Potassium tert-butoxide

生成物 1

HCID 11815890HCID 11815890、化合物収率 55%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A suspension of potassium t-butoxide (60.2 g, 0.54 mole) in toluene is treated with 2,2-dimethyladiponitrile (120.7 g, 0.87 mole) at 80° C., stirred for 2 hours, cooled to less than 30° C., and quenched with water. The phases are separated, the organic phase is stirred with 3N hydrochloric acid and filtered. The filtrate is concentrated in vacuo to give an oil which is distilled (2 torr, 150° C.) twice to afford the title product as a colorless oil, 65.7 g (98.5% pure, 55% yield), identified by gas chromatography.

後処理

  1. temperaturecooled to less than 30° C.
  2. customquenched with water
  3. customThe phases are separated
  4. stirringthe organic phase is stirred with 3N hydrochloric acid
  5. filtrationfiltered
  6. concentrationThe filtrate is concentrated in vacuo
  7. customto give an oil which
  8. distillationis distilled (2 torr, 150° C.) twice

出典と根拠

ORDレコード
ord-4ef161acf469414ba17ef971bbc10a74
出典データセット
uspto-grants-2002_02
特許番号
US06344580B1

反応ノート

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