Acetic Anhydride → HCID 14789836、化合物

HRID 628554

反応式

HRID 628554 の反応式
[C:1]12([OH:13])[CH2:10][C:5]3([OH:11])[CH2:6][CH:7]([CH2:9][C:3]([OH:12])([CH2:4]3)[CH2:2]1)[CH2:8]2.C(O[C:18](=[O:20])[CH3:19])(=O)C>S(=O)(=O)(O)O>[C:5]([O:13][C:1]12[CH2:10][C:5]3([O:11][C:3](=[O:12])[CH3:2])[CH2:6][CH:7]([CH2:9][C:3]([O:12][C:18](=[O:20])[CH3:19])([CH2:4]3)[CH2:2]1)[CH2:8]2)(=[O:11])[CH3:4]

参加物

4

反応物 2

HCID 7918Acetic AnhydrideHCID 98990221,3,5-Adamantanetriol

生成物 1

HCID 14789836HCID 14789836、化合物

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid触媒

反応条件

温度
100 °C

実験手順

92.12 g (0.5 mol) of 1,3,5-adamantanetriol are suspended in 153.14 g (1.5 mol) of acetic anhydride. Subsequently, 10 drops of concentrated sulfuric acid are added and the mixture is stirred on a rotary evaporator (without vacuum) until a homogeneous solution has formed. Subsequently, the mixture is heated to 100° C. under reflux for 2 h. After cooling, the reaction mixture is added to 300 ml of ice-water and extracted with dichloromethane. The combined organic phases are deacidified with sodium carbonate solution and washed with water. The mixture is dried over magnesium sulfate and filtered, and the solvent is removed under reduced pressure. 150.50 g (0.48 mol; 97.0%) of a colorless oil are obtained.

後処理

  1. customhas formed
  2. temperatureunder reflux for 2 h
  3. temperatureAfter cooling
  4. extractionextracted with dichloromethane
  5. washwashed with water
  6. dry with materialThe mixture is dried over magnesium sulfate
  7. filtrationfiltered
  8. customthe solvent is removed under reduced pressure
  9. custom150.50 g (0.48 mol; 97.0%) of a colorless oil are obtained

出典と根拠

ORDレコード
ord-8407d9215afd483db461ba8f7c5e69fb
出典データセット
uspto-grants-2016_04
特許番号
US09314408B2

関連ノート

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