4(2H)-Benzofuranone, 2-ethoxy-3,5,6,7-tetrahydro- → HCID 68282353、化合物
反応式
[CH2:1]([O:3][CH:4]1[CH2:8][C:7]2[C:9](=[O:13])[CH2:10][CH2:11][CH2:12][C:6]=2[O:5]1)[CH3:2]>CCOC(C)=O.[Pd]>[CH2:1]([O:3][CH:4]1[CH2:8][CH:7]2[C:9](=[O:13])[CH2:10][CH2:11][CH2:12][CH:6]2[O:5]1)[CH3:2]参加物
4
実験手順
To a solution of the ketone 10 (140 mg, 0.77 mmol) in EtOAc (9 mL) was added 5% Pd/C (128 mg, 60 μmol) and the mixture was stirred under H2 (1 atm) for 1.5 h at room temperature. The mixture was then filtered on Celite and the pad washed with EtOAc. Evaporation of the solvent furnished the corresponding crude ketone 11 as an essentially pure mixture of diastereoisomers (130 mg, dr=9:1). The ketone was directly submitted to the next step without purification. TLC Major isomer: Rf=0.35 (hexanes:EtOAc=2:1).
後処理
- filtrationThe mixture was then filtered on Celite
- washthe pad washed with EtOAc
- customEvaporation of the solvent
出典と根拠
- ORDレコード
- ord-05d8086049b249f9a5fee86916f433c0
- 出典データセット
- uspto-grants-2015_05
- 特許番号
- US09024038B2
反応ノート
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