Water → 2,2-Dimethylmalonic acid mono-(2,2-dimethylpropyl)ester

HRID 2089663

反応式

HRID 2089663 の反応式
[CH3:1][C:2]([CH3:18])([CH3:17])[CH2:3][O:4][C:5](=[O:16])[C:6]([CH3:15])([CH3:14])[C:7]([O:9]C(C)(C)C)=[O:8].C(OCC)(=O)C.O>ClCCl.C(O)(C(F)(F)F)=O>[CH3:1][C:2]([CH3:18])([CH3:17])[CH2:3][O:4][C:5](=[O:16])[C:6]([CH3:15])([CH3:14])[C:7]([OH:9])=[O:8]

参加物

6

反応物 3

HCID 962WaterHCID 8857Ethyl AcetateHCID 866773992,2-Dimethylmalonic acid t-butyl ester (2,2-dimethylpropyl)ester

生成物 1

HCID 183316662,2-Dimethylmalonic acid mono-(2,2-dimethylpropyl)ester収率 92.6%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 6422Trifluoroacetic acid溶媒

実験手順

To a solution of the obtained 2,2-dimethylmalonic acid t-butyl ester (2,2-dimethylpropyl)ester (12 g) in dichloromethane (100 mL), TFA (20 mL) was added, and the resulting mixture was stirred at room temperature for 3 hours. Ethyl acetate and water were added to the mixture. After shaking the resulting mixture, the organic layer was collected, sequentially washed with water and saturated aqueous sodium chloride solution, and dried over anhydrous magnesium sulfate. The desiccant was filtered off, and toluene was added to the filtrate obtained, after which the resulting mixture was concentrated under reduced pressure to obtain the captioned compound (8.7 g).

後処理

  1. stirringAfter shaking the resulting mixture
  2. customthe organic layer was collected
  3. washsequentially washed with water and saturated aqueous sodium chloride solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationThe desiccant was filtered off
  6. additiontoluene was added to the filtrate
  7. customobtained
  8. concentrationafter which the resulting mixture was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-52d169c4c3d346a2b900021cddd8b91e
出典データセット
uspto-grants-2013_05
特許番号
US08436009B2

関連ノート

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