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

HRID 2089663

반응식

HRID 2089663 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 6422Trifluoroacetic acid용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-52d169c4c3d346a2b900021cddd8b91e
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08436009B2

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