Acetyl chloride → 1-(3,3-Dimethyl-6-nitroindolin-1-yl)ethanone
反応式
[CH3:1][C:2]1([CH3:14])[C:10]2[C:5](=[CH:6][C:7]([N+:11]([O-:13])=[O:12])=[CH:8][CH:9]=2)[NH:4][CH2:3]1.[C:15](Cl)(=[O:17])[CH3:16]>C(Cl)Cl.CCN(CC)CC>[CH3:1][C:2]1([CH3:14])[C:10]2[C:5](=[CH:6][C:7]([N+:11]([O-:13])=[O:12])=[CH:8][CH:9]=2)[N:4]([C:15](=[O:17])[CH3:16])[CH2:3]1参加物
5
実験手順
To a stirred solution of 3,3-dimethyl-6-nitroindoline (450 mg) in CH2Cl2 (15 mL) and Et3N (0.6 mL) at −10° C. was added acetyl chloride (180 μL, 2.5 mmol). The mixture was stirred at rt overnight and quenched by addition of sat. aq. NaHCO3, and extracted with EtOAc (30 mL×3). The combined organic layers were washed with brine, dried (MgSO4) and concentrated. The residue was purified by column to give a light yellow solid (390 mg, 71% for two steps).
後処理
- customquenched by addition of sat. aq. NaHCO3
- extractionextracted with EtOAc (30 mL×3)
- washThe combined organic layers were washed with brine
- dry with materialdried (MgSO4)
- concentrationconcentrated
- customThe residue was purified by column
- customto give a light yellow solid (390 mg, 71% for two steps)
出典と根拠
- ORDレコード
- ord-69bb6cf137814da0ad45c73203248933
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07745451B2
反応ノート
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