Methyl iodide → HCID 14732816、化合物
反応式
[C:1]1(=[O:10])[C:6]2[CH2:7][CH2:8][CH2:9][C:5]=2[CH:4]=[CH:3][NH:2]1.[H-].[Na+].[CH3:13]I>CN(C=O)C>[CH3:13][N:2]1[CH:3]=[CH:4][C:5]2[CH2:9][CH2:8][CH2:7][C:6]=2[C:1]1=[O:10]参加物
5
反応条件
- 温度
- 0 °C
実験手順
The title compound of step 5 (260 mg, 1.93 mmol) was dissolved in DMF (5 mL) and cooled to 0° C. NaH (94 mg, 2.31 mmol) was added and the mixture was stirred for 30 min. Methyl iodide (146 μL, 2.31 mmol) was added and the mixture stirred at rt for 2 h. The volatile components were removed under vacuum and silica gel chromatography (PE/EtOAc=1:1) gave the title compound (192.6 mg, 67%) as a brown oil. 1H NMR (CD3Cl, 300 MHz): δ 7.13 (d, J=6.6 Hz, 1H), 6.13 (d, J=6.6 Hz, 1H), 3.53 (s, 3H), 2.79-2.85 (m, 4H), 2.01-2.11 (m, 2H). LCMS: 150 (M+1)+
後処理
- stirringthe mixture stirred at rt for 2 h
- customThe volatile components were removed under vacuum and silica gel chromatography (PE/EtOAc=1:1)
出典と根拠
- ORDレコード
- ord-cac1da1be2b14722a803c924a876d845
- 出典データセット
- uspto-grants-2015_08
- 特許番号
- US09115114B2
反応ノート
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