Sodium Hydroxide → 7-(2,5-Dimethoxy-3,4,6-trimethylphenyl)-2,2-dimethyl-7-phenylheptanoic acid

HRID 1646825

반응식

HRID 1646825 반응식
[OH-].[Na+].[CH3:3][O:4][C:5]1[C:10]([CH3:11])=[C:9]([CH3:12])[C:8]([O:13][CH3:14])=[C:7]([CH3:15])[C:6]=1[CH:16]([C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)[CH2:17][CH2:18][CH2:19][CH2:20][C:21]([CH3:28])([CH3:27])[C:22]([O:24]CC)=[O:23]>C(O)C>[CH3:3][O:4][C:5]1[C:10]([CH3:11])=[C:9]([CH3:12])[C:8]([O:13][CH3:14])=[C:7]([CH3:15])[C:6]=1[CH:16]([C:29]1[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=1)[CH2:17][CH2:18][CH2:19][CH2:20][C:21]([CH3:28])([CH3:27])[C:22]([OH:24])=[O:23]

참가 물질

4

반응 조건

온도
90 °C

실험 절차

3N Sodium hydroxide (9 ml) was added to a solution of 1.20 g (2.73 mmole) of ethyl 7-(2,5-dimethoxy-3,4,6-trimethylphenyl)-2,2-dimethyl-7-phenylheptanoate in ethanol (12 ml), followed by stirring at 90° C. overnight (15 hours). After cooling by standing at room temperature, the ethanol was distilled off under reduced pressure, and the residue was made acid by adding a 10% aqueous phosphoric acid solution, followed by extraction of the product with isopropyl ether. The isopropyl ether layer was washed with aqueous sodium hydrochloride solution, dried (magnesium suflate) and evaporated to give 1.11 q (99%) of 7-(2,5-dimethoxy-3,4,6-trimethylphenyl)-2,2-dimethyl-7-phenylheptanoic acid. Its typical physical properties and nuclear magnetic resonance spectrum data are shown in Table 14.

후처리

  1. temperatureAfter cooling
  2. customby standing at room temperature
  3. distillationthe ethanol was distilled off under reduced pressure
  4. additionby adding a 10% aqueous phosphoric acid solution
  5. extractionfollowed by extraction of the product with isopropyl ether
  6. washThe isopropyl ether layer was washed with aqueous sodium hydrochloride solution
  7. dry with materialdried (magnesium suflate)
  8. customevaporated

출처 및 근거

ORD 기록
ord-159e3818d89848a4bed8302dc9d8b313
출처 데이터셋
uspto-grants-1993_01
특허 번호
US05180742

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