Formamide → 4-Methoxyisoindoline-1,3-dione
反応式
[CH3:1][O:2][C:3]1[CH:13]=[CH:12][CH:11]=[C:5]2[C:6]([O:8][C:9](=O)[C:4]=12)=[O:7].C([NH2:16])=O>O>[CH3:1][O:2][C:3]1[CH:13]=[CH:12][CH:11]=[C:5]2[C:6]([NH:16][C:9](=[O:8])[C:4]=12)=[O:7]参加物
4
実験手順
A mixture of 3-methoxyphthalic anhydride (24.0 g, 134.8 mmol) and formamide (120 ml) was stirred and held at 210° C. for 5 hours and was then allowed to cool to room temperature overnight. Water (100 ml) was added and the solid material filtered off under reduced pressure. The crude product was washed sequentially with 50% aqueous acetone (50 ml) and diethyl ether (200 ml) and sucked dry under reduced pressure to afford 3-methoxyphthalimide (8.95 g, 37%) as an off-white solid. 1H NMR (DMSO-d6) 11.08 (1H, br s), 7.78 (1H, dd), 7.45 (1H, d), 7.36 (1H, d), 3.93 (3H, s). MS: [M+H]+ 178.
後処理
- filtrationthe solid material filtered off under reduced pressure
- washThe crude product was washed sequentially with 50% aqueous acetone (50 ml) and diethyl ether (200 ml)
- customsucked dry under reduced pressure
出典と根拠
- ORDレコード
- ord-ded08a33f7ef4150b3184e5faa2faedc
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08530469B2
反応ノート
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