Ammonia → [(2S)-5-Fluoro-7-(methylsulfonyl)-2,3-dihydro-1,4-benzodioxin-2-YL]methylamine
反応式
CC1C=CC(S(O[CH2:12][C@@H:13]2[O:18][C:17]3[CH:19]=[C:20]([S:24]([CH3:27])(=[O:26])=[O:25])[CH:21]=[C:22]([F:23])[C:16]=3[O:15][CH2:14]2)(=O)=O)=CC=1.[NH3:28]>>[F:23][C:22]1[C:16]2[O:15][CH2:14][C@H:13]([CH2:12][NH2:28])[O:18][C:17]=2[CH:19]=[C:20]([S:24]([CH3:27])(=[O:26])=[O:25])[CH:21]=1参加物
3
反応条件
- 温度
- 120 °C
実験手順
A mixture of [(2R)-5-fluoro-7-(methylsulfonyl)-2,3-dihydro-1,4-benzodioxin-2-yl]methyl 4-methylbenzenesulfonate (0.7 g, 1.7 mmol), NH3 (6 ml, 7N in methanol) was heated under microwave radiation at 120° C. for 20 min. The product was evaporated to dryness and was purified on an SCX-3 column (TEA/MeOH) Yield 0.34 g. MS m/z (rel. intensity, 70 eV) 261 (M+, bp), 217 (49), 97 (39), 69 (55), 56 (79).
後処理
- customThe product was evaporated to dryness
- customwas purified on an SCX-3 column (TEA/MeOH) Yield 0.34 g
出典と根拠
- ORDレコード
- ord-0ecd56fbc85842d2b8aad7006a6ce224
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08524766B2
反応ノート
読み込み中…