Water → HCID 86733843、化合物

HRID 2072004ノート

反応式

HRID 2072004 の反応式
[CH2:1]([CH2:8][NH:9][C:10]([CH3:14])([CH3:13])[C:11]#[N:12])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O>CCOCC>[CH2:1]([CH2:8][NH:9][C:10]([CH3:14])([CH3:13])[CH2:11][NH2:12])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 962WaterHCID 214098442-Benzylmethylamino-2-methylpropionitrile

生成物 1

HCID 86733843HCID 86733843、化合物収率 55.5%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

A solution of 2-benzylmethylamino-2-methylpropionitrile (6.7 g.) in ether (100 ml.) was added dropwise to a stirred solution of sodium dihydro bis[2-methoxyethoxy] aluminate (28.5 g.) in ether (150 ml.), kept at 0° C. The mixture was then gently refluxed for 20 hrs, and then excess reducing agent was decomposed by the dropwise addition of water to the cooled suspension. The mixture was dried (anhyd.Na2SO4), filtered (hyflo) and the excess ether evaporated under reduced pressure. The residual liquid was distilled under water pump vacuum to give 2-benzylmethylamino-2-methyl-propylamine (3.8 g.) b.p. 138°-140° C.

後処理

  1. customkept at 0° C
  2. temperatureThe mixture was then gently refluxed for 20 hrs
  3. dry with materialThe mixture was dried (anhyd.Na2SO4)
  4. filtrationfiltered (hyflo)
  5. customthe excess ether evaporated under reduced pressure
  6. distillationThe residual liquid was distilled under water

出典と根拠

ORDレコード
ord-6d48ec0a115741d484345948ad46325e
出典データセット
uspto-grants-1977_09
特許番号
US04049663

反応ノート

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