6-Hydroxy-3-methyl-4-vinyl-phthalic Acid Dimethyl Ester → 4-Ethyl-6-hydroxy-3-methyl-phthalic Acid Dimethyl Ester

HRID 272194

반응식

HRID 272194 반응식
[CH3:1][O:2][C:3](=[O:18])[C:4]1[C:5](=[C:10]([CH3:17])[C:11]([CH:15]=[CH2:16])=[CH:12][C:13]=1[OH:14])[C:6]([O:8][CH3:9])=[O:7]>C1C=CC=CC=1.CCOC(C)=O>[CH3:1][O:2][C:3](=[O:18])[C:4]1[C:5](=[C:10]([CH3:17])[C:11]([CH2:15][CH3:16])=[CH:12][C:13]=1[OH:14])[C:6]([O:8][CH3:9])=[O:7]

참가 물질

4

반응물 1

HCID 597944986-Hydroxy-3-methyl-4-vinyl-phthalic Acid Dimethyl Ester

생성물 1

HCID 597944774-Ethyl-6-hydroxy-3-methyl-phthalic Acid Dimethyl Ester수율 88.4%

시약·촉매·용매 2

HCID 241Benzene용매HCID 8857Ethyl Acetate용매

실험 절차

6-Hydroxy-3-methyl-4-vinyl-phthalic acid dimethyl ester (1.27 g, 5.11 mmol) was dissolved in benzene (10 mL) and EtOAc (10 mL). Tristriphenylphosphine rhodium chloride (150 mg) was added and the reaction was placed under an atmosphere of hydrogen. Stirring at room temperature was continued. After 14 hours, the solvents were removed in vacuo and the crude material was purified by silica gel chromatography to provide 1.14 g (88%) of the desired product as an off-white solid. 1H NMR (300 MHz, CDCl3): δ=1.19 (t, J=7.8 Hz, 3H), 2.10 (s, 3H), 2.60 (q, J=7.8 Hz, 2H), 3.89 (s, 6H), 6.87 (s, 1H), 10.79 (s, 1H) ppm.

후처리

  1. customthe solvents were removed in vacuo
  2. customthe crude material was purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-f030c0e328744626b6a9d1e4a949d794
출처 데이터셋
uspto-grants-2008_11
특허 번호
US07452901B2

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