Isopropanol → 1-((2-Chloro-5-fluoropyrimidin-4-ylamino)methyl)cyclohexanol
反応式
Cl.[NH2:2][CH2:3][CH:4]1[CH2:9][CH2:8][CH2:7][CH2:6][CH:5]1O.[Cl:11][C:12]1[N:17]=[C:16](Cl)[C:15]([F:19])=[CH:14][N:13]=1.CCN(C(C)C)C(C)C.C([OH:32])(C)C>>[Cl:11][C:12]1[N:17]=[C:16]([NH:2][CH2:3][C:4]2([OH:32])[CH2:9][CH2:8][CH2:7][CH2:6][CH2:5]2)[C:15]([F:19])=[CH:14][N:13]=1参加物
5
反応条件
- 温度
- 80 °C
実験手順
To a solution of 2-(aminomethyl)cyclohexanol hydrochloride (0.09 g, 0.54 mmol) and 2,4-dichloro-5-fluoro-pyrimidine (0.10 g, 0.60 mmol) in isopropanol (2 mL) was added iPr2NEt (0.21 mL, 1.20 mmol). The reaction mixture was heated at 80° C. for 12 hours. The reaction mixture was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography (25%-75% EtOAc/hexanes) to afford desired product, 14a.
後処理
- concentrationThe reaction mixture was concentrated under reduced pressure
- customthe resulting residue was purified by silica gel chromatography (25%-75% EtOAc/hexanes)
出典と根拠
- ORDレコード
- ord-f6b051ef2dc44a4d8d273467548736ef
- 出典データセット
- uspto-grants-2016_05
- 特許番号
- US09345708B2
反応ノート
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