Acetic Anhydride → HCID 14789836, 화합물

HRID 628554

반응식

HRID 628554 반응식
[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]

참가 물질

4

반응물 2

HCID 7918Acetic AnhydrideHCID 98990221,3,5-Adamantanetriol

생성물 1

HCID 14789836HCID 14789836, 화합물

시약·촉매·용매 1

HCID 1118Sulfuric Acid촉매

반응 조건

온도
100 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8407d9215afd483db461ba8f7c5e69fb
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09314408B2

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