Ethylene Glycol → HCID 21520276, 화합물

HRID 1282828노트

반응식

HRID 1282828 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

HCID 21520276HCID 21520276, 화합물수율 78.8%

시약·촉매·용매 2

HCID 6101p-Toluenesulfonic acid촉매HCID 1140Toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3d961d26fdb64c97a62727b4d0e534cf
출처 데이터셋
uspto-grants-1976_08
특허 번호
US03972900

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