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

HRID 963721ノート

反応式

HRID 963721 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-41a49a8cfdbf4633b22ac1225d9bdc64
出典データセット
uspto-grants-1998_06
特許番号
US05763489

反応ノート

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