Acetic Anhydride → HCID 21498552、化合物

HRID 1729967ノート

反応式

HRID 1729967 の反応式
[CH3:1][C:2]12[CH2:10][CH2:9][CH:5]([CH:6]([OH:8])[CH2:7]1)[C:4]([CH3:12])([CH3:11])[NH:3]2.[C:13](OC(=O)C)(=[O:15])[CH3:14]>C(O)(=O)C>[C:13]([O:8][CH:6]1[CH2:7][C:2]2([CH3:1])[CH2:10][CH2:9][CH:5]1[C:4]([CH3:12])([CH3:11])[NH:3]2)(=[O:15])[CH3:14]

参加物

4

反応物 2

HCID 7918Acetic AnhydrideHCID 214985461,3,3-Trimethyl-2-azabicyclo[2.2.2]octan-5-ol

生成物 1

HCID 21498552HCID 21498552、化合物収率 36.4%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

To a solution of 1.8 g (0.016 moles) of 1,3,3-trimethyl-2-azabicyclo[2.2.2]octane-5ol in 30 ml of glacial acetic acid in a 100 ml flask equipped with a magnetic stirrer, thermometer, condenser, and drying tube was added 1.0 ml (0.106 moles) of acetic anhydride. The solution was boiled under reflux for 20 hours. The reaction mixture was then cooled and evaporated under reduced pressure. The residue was taken up in hexane, and allowed to stand at room temperature overnight. The solution was then filtered and the filtrate evaporated under reduced pressure and dried under vacuum at 35° C, yielding 1.23 g of the desired material as a colorless oil.

後処理

  1. customthermometer, condenser, and drying tube
  2. temperatureunder reflux for 20 hours
  3. temperatureThe reaction mixture was then cooled
  4. customevaporated under reduced pressure
  5. filtrationThe solution was then filtered
  6. customthe filtrate evaporated under reduced pressure
  7. customdried under vacuum at 35° C

出典と根拠

ORDレコード
ord-766a183fd5d74534b206f9f38d3b7579
出典データセット
uspto-grants-1976_11
特許番号
US03991012

反応ノート

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