1,4-Dioxane hydrochloride → (2R)-N-cyclopropyl-N-{(1R)-1-[1-(3-methoxypropyl)-3-methyl-1H-indazol-6-yl]ethyl}morpholine-2-carboxamide hydrochloride
反応式
[CH:1]1([N:4]([C@@H:20]([C:22]2[CH:30]=[C:29]3[C:25]([C:26]([CH3:36])=[N:27][N:28]3[CH2:31][CH2:32][CH2:33][O:34][CH3:35])=[CH:24][CH:23]=2)[CH3:21])[C:5]([C@@H:7]2[O:12][CH2:11][CH2:10][N:9](C(OC(C)(C)C)=O)[CH2:8]2)=[O:6])[CH2:3][CH2:2]1.[ClH:37].O1CCOCC1>C(Cl)(Cl)Cl>[ClH:37].[CH:1]1([N:4]([C@@H:20]([C:22]2[CH:30]=[C:29]3[C:25]([C:26]([CH3:36])=[N:27][N:28]3[CH2:31][CH2:32][CH2:33][O:34][CH3:35])=[CH:24][CH:23]=2)[CH3:21])[C:5]([C@@H:7]2[O:12][CH2:11][CH2:10][NH:9][CH2:8]2)=[O:6])[CH2:3][CH2:2]1参加物
4
実験手順
To a solution of tert-butyl (2R)-2-[(cyclopropyl{(1R)-1-[1-(3-methoxypropyl)-3-methyl-1H-indazol-6-yl]ethyl}amino)carbonyl]morpholine-4-carboxylate (44.4 mg) in chloroform (2.0 mL) was added 4-normal hydrogen chloride-dioxane solution (0.75 mL) under ice-cooling, and the mixture was stirred at room temperature for 20 hours. The reaction solution was concentrated under reduced pressure, and the resulting residue was dissolved in water (1 mL), and then washed with diethyl ether. The aqueous layer was freeze-dried to give (2R)-N-cyclopropyl-N-{(1R)-1-[1-(3-methoxypropyl)-3-methyl-1H-indazol-6-yl]ethyl}morpholine-2-carboxamide hydrochloride [Ex(3-1)] (25 mg) as a colorless powder.
後処理
- temperaturecooling
- concentrationThe reaction solution was concentrated under reduced pressure
- dissolutionthe resulting residue was dissolved in water (1 mL)
- washwashed with diethyl ether
- customThe aqueous layer was freeze-dried
出典と根拠
- ORDレコード
- ord-417c31e79b1d4b73a77f468eba88e839
- 出典データセット
- uspto-grants-2016_03
- 特許番号
- US09278944B2
反応ノート
読み込み中…