Ethylene Glycol → HCID 54259475、化合物

HRID 1758263ノート

反応式

HRID 1758263 の反応式
[CH:1]([CH:4]([C:7]1[CH:15]=[CH:14][C:10]2[CH:11]=[CH:12][O:13][C:9]=2[CH:8]=1)[C:5]#N)([CH3:3])[CH3:2].[OH-:16].[K+].C(O)C[OH:20]>O>[CH:1]([CH:4]([C:7]1[CH:15]=[CH:14][C:10]2[CH:11]=[CH:12][O:13][C:9]=2[CH:8]=1)[C:5]([OH:20])=[O:16])([CH3:3])[CH3:2]

参加物

5

反応物 3

HCID 174Ethylene GlycolHCID 14797Potassium HydroxideHCID 54066355HCID 54066355、化合物

生成物 1

HCID 54259475HCID 54259475、化合物収率 50.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
140 °C

実験手順

A mixture of α-isopropylbenzofuran-6-acetonitrile (1.62 g, 0.008 mol), potassium hydroxide (2.29 g, 0.039 mol), ethane-1,2-diol (28 cm3) and water (2.3 cm3) was refluxed at 140° C. for 18 hr. The cooled mixture was poured into water and extracted with diethyl ether. The aqueous solution was acidified with hydrochloric acid and the mixture was extracted with diethyl ether. The ether extract was washed with water, dried (Na2SO4), filtered and the solvent was removed to give α-isopropylbenzofuran-6-acetic acid (0.90 g, 0.0041 mol, 50.8%). Recrystallised from petroleum ether (b.p. 60°-80° C.) m.p. 99°-100° C. (Found: C, 71.52; H, 6.65; C13H14O3 requires C, 71.54; H, 6.47%), t.l.c./silica/ethyl acetate RF 0.40.

後処理

  1. extractionextracted with diethyl ether
  2. extractionthe mixture was extracted with diethyl ether
  3. extractionThe ether extract
  4. washwas washed with water
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. customthe solvent was removed

出典と根拠

ORDレコード
ord-4c00e3c704d840b78106dd02db71ab06
出典データセット
uspto-grants-1983_02
特許番号
US04372970

反応ノート

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