Water → 2-Methyl-2-methoxycarbonyl-5-methoxy-1,2,3,4-tetrahydronaphthalene

HRID 963721노트

반응식

HRID 963721 반응식
[CH3:1][C:2]1([C:15]([O:17][CH3:18])=[O:16])[CH2:11][CH2:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][C:8]=2[O:12][CH3:13])[C:3]1=O.C([SiH](CC)CC)C.C(OCC)(=O)C.O>FC(F)(F)C(O)=O>[CH3:1][C:2]1([C:15]([O:17][CH3:18])=[O:16])[CH2:11][CH2:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][C:8]=2[O:12][CH3:13])[CH2:3]1

참가 물질

6

반응물 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 12052TriethylsilaneHCID 543642852-Methyl-2-methoxycarbonyl-5-methoxy-1-oxo-1,2,3,4-tetrahydronaphthalene

생성물 1

HCID 540790102-Methyl-2-methoxycarbonyl-5-methoxy-1,2,3,4-tetrahydronaphthalene수율 211.9%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

To a solution of 2-methyl-2-methoxycarbonyl-5-methoxy-1-oxo-1,2,3,4-tetrahydronaphthalene (2.0 g) in trifluoroacetic acid (20 ml) was added triethylsilane (2.0 ml) at room temperature. After being stirred for 6 hours at room temperature, the solution was poured into a mixture of ethyl acetate and water. The organic layer was washed with 1N--HCl solution, sat. NaHCO3, and brine, dried over MgSO4, and evaporated in vacuo. The residue was purified by chromatography on silica gel to afford 2-methyl-2-methoxycarbonyl-5-methoxy-1,2,3,4-tetrahydronaphthalene (4.0 g).

후처리

  1. washThe organic layer was washed with 1N
  2. dry with materialHCl solution, sat. NaHCO3, and brine, dried over MgSO4
  3. customevaporated in vacuo
  4. customThe residue was purified by chromatography on silica gel

출처 및 근거

ORD 기록
ord-41a49a8cfdbf4633b22ac1225d9bdc64
출처 데이터셋
uspto-grants-1998_06
특허 번호
US05763489

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