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Ethyl p-methylbenzenesulfonate → 3-Ethoxy-2,2-dimethylpropionic acid methyl ester

HRID 2200783
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HRID 2200783 반응식
[H-].[Na+].[CH3:3][O:4][C:5](=[O:11])[C:6]([CH3:10])([CH3:9])[CH2:7][OH:8].[CH2:12](OS(C1C=CC(C)=CC=1)(=O)=O)[CH3:13]>CN(C)C=O.O.CCCCCC>[CH3:3][O:4][C:5](=[O:11])[C:6]([CH3:10])([CH3:9])[CH2:7][O:8][CH2:12][CH3:13]
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참가 물질

6

반응물 3

HCID 6638Ethyl p-methylbenzenesulfonateHCID 24758Sodium hydrideHCID 84152Methyl 3-hydroxypivalate

생성물 1

HCID 592680143-Ethoxy-2,2-dimethylpropionic acid methyl ester수율 34%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매2회HCID 22114717
Water hexane
용매

실험 절차

1 mol of sodium hydride was added to the solvent dimethylformamide, and 1 mol of hydroxypivalic acid methyl ester was added thereto while the temperature of the solution did not exceed 30° C. The solution was stirred at room temperature for 90 minutes. Then, 1.2 mol of p-toluenesulfonic acid ethyl ester was added to the solution while the temperature of the solution did not exceed 30° C. Then, a water/hexane mixture having the same mass as that of the dimethylformamide was added to and mixed with the solution, after which water was removed therefrom. The resulting organic material was concentrated, and the residue was fractionated at atmospheric pressure and 108˜111° C., thereby obtaining the intermediate 3-ethoxy-2,2-dimethylpropionic acid methyl ester at a yield of 34%.

후처리

  1. additionwas added
  2. customdid not exceed 30° C
  3. customdid not exceed 30° C
  4. additionwas added to and
  5. additionmixed with the solution
  6. customafter which water was removed
  7. concentrationThe resulting organic material was concentrated
  8. customwas fractionated at atmospheric pressure and 108˜111° C.

출처 및 근거

ORD 기록
ord-b457c3fd8b80449e9cb6faa4e712ec8b
출처 데이터셋
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09359382B2

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