Ethanolamine → N-(2-Hydroxyethyl)-2-(isopropyl)-5-methylcyclohexanecarboxamide

HRID 26386ノート

反応式

HRID 26386 の反応式
[CH:1]1([CH3:13])[CH2:6][CH2:5][CH:4]([CH:7]([CH3:9])[CH3:8])[CH:3]([C:10](Cl)=[O:11])[CH2:2]1.[CH2:14]([CH2:16][NH2:17])[OH:15]>C(Cl)(Cl)Cl>[OH:15][CH2:14][CH2:16][NH:17][C:10]([CH:3]1[CH:4]([CH:7]([CH3:9])[CH3:8])[CH2:5][CH2:6][CH:1]([CH3:13])[CH2:2]1)=[O:11]

参加物

4

反応物 2

HCID 700EthanolamineHCID 13734319Cyclohexanecarbonyl chloride, 5-methyl-2-(1-methylethyl)-

生成物 1

HCID 3016102N-(2-Hydroxyethyl)-2-(isopropyl)-5-methylcyclohexanecarboxamide

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

A solution of p-menth-3-oyl chloride prepared as in Example 1 (4.0g., 0.020 moles) in chloroform (30 ml.) was added dropwise to a stirred solution of ethanolamine (3 g., 0.043 moles) in chloroform (50 ml.). The reaction mixture becomes warm, goes cloudy and finally a yellow oil starts to separate out. After stirring for 2 hours at room temperature the mixture was poured into water. The organic layer was separated, washed with dilute H2SO4, and dried (MgSO4). Removal of the solvent left a viscous oil (3.8 g.). This was distilled under vacuum to yield N-(2-hydroxyethyl)-p-menthane-3-carboxamide as a colourless very viscous oil, b.p. 160°/01. mm.

後処理

  1. temperatureThe reaction mixture becomes warm
  2. customfinally a yellow oil starts to separate out
  3. additionwas poured into water
  4. customThe organic layer was separated
  5. washwashed with dilute H2SO4
  6. dry with materialdried (MgSO4)
  7. customRemoval of the solvent
  8. waitleft a viscous oil (3.8 g.)
  9. distillationThis was distilled under vacuum

出典と根拠

ORDレコード
ord-d4a83106185d4c60b359d7037c4b05d9
出典データセット
uspto-grants-1979_04
特許番号
US04150052

反応ノート

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