Hydrochloric Acid → 3-(3-hydroxymethyl-phenyl)-4H-[1,2,4]oxadiazol-5-one
反応式
Cl.O1CCCCC1[O:8][CH2:9][C:10]1[CH:11]=[C:12]([C:16]2[NH:20][C:19](=[O:21])[O:18][N:17]=2)[CH:13]=[CH:14][CH:15]=1>O1CCCC1.[Cl-].[Na+].O>[OH:8][CH2:9][C:10]1[CH:11]=[C:12]([C:16]2[NH:20][C:19](=[O:21])[O:18][N:17]=2)[CH:13]=[CH:14][CH:15]=1参加物
5
実験手順
Add 10% hydrochloric acid (100 ml) to a solution of 3-[3-(tetrahydro-pyran-2-yloxymethyl)-phenyl]-4H-[1,2,4]oxadiazol-5-one (4.50 g, 16.3 mmol) in tetrahydrofuran (0.1M) and stir. After 18 hours, pour reaction into brine and extract with ethyl acetate. Combine the organic layers, dry with sodium sulfate, filter and concentrate under reduced pressure to yield the title product as a white solid (3.10 g, 99%): 1H NMR (DMSO-d6) δ 4.57 (s, 2H), 7.55 (m, 2H), 7.67 (dt, 1H), 7.81 (m, 1H), 12.95 (bs, 1H).
後処理
- additionpour
- extractionextract with ethyl acetate
- dry with materialdry with sodium sulfate
- filtrationfilter
- concentrationconcentrate under reduced pressure
出典と根拠
- ORDレコード
- ord-22ac86b5431142559d871884194d6cd2
- 出典データセット
- uspto-grants-2009_10
- 特許番号
- US07598423B2
反応ノート
読み込み中…