Ethylene Glycol → HCID 21520276、化合物

HRID 1282828ノート

反応式

HRID 1282828 の反応式
[C:1]([C:4]1[O:5][C:6]2[C:12]([CH2:13][CH3:14])=[CH:11][CH:10]=[CH:9][C:7]=2[CH:8]=1)(=[O:3])[CH3:2].[CH2:15](O)[CH2:16][OH:17].O>C1(C)C=CC=CC=1.C1(C)C=CC(S(O)(=O)=O)=CC=1>[CH2:13]([C:12]1[C:6]2[O:5][C:4]([C:1]3([CH3:2])[O:17][CH2:16][CH2:15][O:3]3)=[CH:8][C:7]=2[CH:9]=[CH:10][CH:11]=1)[CH3:14]

参加物

6

反応物 3

HCID 174Ethylene GlycolHCID 962WaterHCID 124484571-(7-Ethyl-1-benzofuran-2-yl)ethan-1-one

生成物 1

HCID 21520276HCID 21520276、化合物収率 78.8%

試薬・触媒・溶媒 2

HCID 6101p-Toluenesulfonic acid触媒HCID 1140Toluene溶媒

実験手順

A stirred mixture of 50 g of 2-acetyl-7-ethylbenzofuran, 3.0 g of paratoluenesulphonic acid and 45.0 g of ethyleneglycol in 1200 ml of toluene was heated under reflux for 12 hours with azeotropic removal of water. The cooled solution was washed successively with dilute sodium hydroxide solution, water and brine and then dried over anhydrous sodium sulphate. The sodium sulphate was filtered off and the filtrate evaporated to dryness. The residual yellow oil was distilled under nitrogen to give 48.6 g of 7-ethyl-2-(2-methyl-1,3-dioxolan-2-yl)benzofuran of boiling point 86°-88°C/0.05 mm Hg.

後処理

  1. temperaturewas heated
  2. washThe cooled solution was washed successively with dilute sodium hydroxide solution, water and brine
  3. dry with materialdried over anhydrous sodium sulphate
  4. filtrationThe sodium sulphate was filtered off
  5. customthe filtrate evaporated to dryness
  6. distillationThe residual yellow oil was distilled under nitrogen

出典と根拠

ORDレコード
ord-3d961d26fdb64c97a62727b4d0e534cf
出典データセット
uspto-grants-1976_08
特許番号
US03972900

反応ノート

読み込み中…