Ethylamine → N-Ethyl-2-isobutyl-2,4-dimethylvaleramide

HRID 262100ノート

反応式

HRID 262100 の反応式
[CH2:1]([C:5]([CH3:13])([CH2:9][CH:10]([CH3:12])[CH3:11])[C:6]([OH:8])=[O:7])[CH:2]([CH3:4])[CH3:3].[CH2:14]([C:16]#[N:17])C.C(Br)C(C)C.S(Cl)([Cl:25])=O.C(N)C>CCOCC.O>[CH2:1]([C:5]([CH3:13])([CH2:9][CH:10]([CH3:12])[CH3:11])[C:6]([Cl:25])=[O:7])[CH:2]([CH3:4])[CH3:3].[CH2:16]([NH:17][C:6](=[O:8])[C:5]([CH2:1][CH:2]([CH3:3])[CH3:4])([CH3:13])[CH2:9][CH:10]([CH3:12])[CH3:11])[CH3:14]

参加物

9

反応物 5

HCID 6341EthylamineHCID 65551-Bromo-2-methylpropaneHCID 7854PropionitrileHCID 24386Thionyl ChlorideHCID 266760HCID 266760、化合物

生成物 2

HCID 3016606N-Ethyl-2-isobutyl-2,4-dimethylvaleramideHCID 20565978HCID 20565978、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 3283Diethyl Ether溶媒2 回

実験手順

2-isobutyl-2,4-dimethylpentanoyl chloride (bp. 97°-100°/16 mm) was prepared in the usual way from 2-isobutyl-2,4-dimethylpentanoic acid (prepared by the alkylation of ethyl cyanide with 2 equivalents of isobutyl bromide, followed by hydrolysis) and thionyl chloride. A solution of the acid chloride (1.5g) in ether (20 ml) was added with stirring to a solution of ethylamine (5ml of a 70% solution in water) in ether (100 ml). After stirring for 2 hours the ethereal layer was washed with dilute hydrochloric acid and water. The dried (MgSO4) ether solution was concentrated and the residue was recrystallised from petroleum ether (bp. 40°-60°) to give N-ethyl-2-isobutyl-2,4-dimethylpentanamide, mp. 71.5°-72.5°.

後処理

  1. washwas washed with dilute hydrochloric acid and water
  2. dry with materialThe dried (MgSO4) ether solution
  3. concentrationwas concentrated
  4. customthe residue was recrystallised from petroleum ether (bp. 40°-60°)

出典と根拠

ORDレコード
ord-b8f0e0b5ac854d018912e316e4755de4
出典データセット
uspto-grants-1979_05
特許番号
US04153679

反応ノート

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