Tetrahydrofuran → HCID 86669311、化合物
反応式
C[O:2][C:3](=[O:20])[C:4]1[CH:9]=[C:8]([N+:10]([O-:12])=[O:11])[C:7]([NH:13]C)=[N:6][C:5]=1[O:15][CH2:16][CH:17]([F:19])[F:18].C1COCC1.[OH-].[Na+]>O>[F:19][CH:17]([F:18])[CH2:16][O:15][C:5]1[N:6]=[C:7]([NH2:13])[C:8]([N+:10]([O-:12])=[O:11])=[CH:9][C:4]=1[C:3]([OH:20])=[O:2]参加物
5
実験手順
A mixture of methyl-2-(2,2-difluoro-ethoxy)-6-methylamino-5-nitro-nicotinate (9.1 g, 32 mmol, prepared according to WO2010/34799), THF (100 mL), water (60 mL) and 1N aq. NaOH-solution (60 mL) is stirred for 3 h at rt, then the mixture is concentrated i.vac. The water phase is washed with Et2O, 60 mL 1N HCl solution is added and the resulting precipitate is collected and dried.
後処理
- concentrationthe mixture is concentrated i.vac
- washThe water phase is washed with Et2O, 60 mL 1N HCl solution
- additionis added
- customthe resulting precipitate is collected
- customdried
出典と根拠
- ORDレコード
- ord-78e8eb5b6896447289695f792af65301
- 出典データセット
- uspto-grants-2013_07
- 特許番号
- US08486968B2
反応ノート
読み込み中…