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

HRID 903310ノート

反応式

HRID 903310 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 (4.0 g., 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-4d0954d73fc345648aec9ed28939f9c4
出典データセット
uspto-grants-1980_10
特許番号
US04226988

反応ノート

読み込み中…