Acetic Acid → HCID 178439162、化合物

HRID 382923

反応式

HRID 382923 の反応式
[C:1]([OH:4])(=O)[CH3:2].[C:5](O)([CH3:8])([CH3:7])[CH3:6].O.[CH2:11]=[C:12]=[O:13].[CH2:14](N(CC)CC)[CH3:15]>>[CH3:6][CH:5]([C:8]1[CH:2]=[C:1]([OH:4])[C:12](=[O:13])[CH:11]=[CH:15][CH:14]=1)[CH3:7]

参加物

6

反応物 5

HCID 176Acetic AcidHCID 962WaterHCID 6386tert-ButanolHCID 8471TriethylamineHCID 10038Ketene2 回

生成物 1

HCID 178439162HCID 178439162、化合物収率 66%

反応条件

温度
60 °C

実験手順

A mixed solvent consisting of 24 g of acetic acid, 377 g of t-butanol and 49 g of water was added to the distillate containing the ketene adducts, and 99 g of triethylamine was added dropwise over a period of 2 hours while maintaining the solution temperature at 60° C. Then, the resulting mixture was heated at 60° C. for another 5 hours. After completion of the reaction, analysis by a gas chromatography revealed that peaks due to the ketene adducts disappeared and that hinokitiol was obtained in 66% yield (0.26 mol).

後処理

  1. additionwas added to the distillate
  2. additionwas added dropwise over a period of 2 hours
  3. temperatureThen, the resulting mixture was heated at 60° C. for another 5 hours
  4. customAfter completion of the reaction, analysis by a gas chromatography

出典と根拠

ORDレコード
ord-140131d9b60e4aab9f931625c05db0da
出典データセット
uspto-grants-2001_10
特許番号
US06310255B1

関連ノート

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