Hydrogen chloride-ethyl acetate → (6r)-6-(Methoxymethyl)-3-[2-(methoxymethyl)pyrrolidin-1-yl]-6,7,8,9-tetrahydropyrazino[2,3-f][1,4]oxazepine hydrochloride
反応式
C([N:8]1[CH2:14][C:13]2[N:15]=[CH:16][C:17]([N:19]3[CH2:23][CH2:22][CH2:21][CH:20]3[CH2:24][O:25][CH3:26])=[N:18][C:12]=2[O:11][C@@H:10]([CH2:27][O:28][CH3:29])[CH2:9]1)C1C=CC=CC=1.C(OCC)(=O)C.[ClH:36]>CO.[OH-].[OH-].[Pd+2]>[ClH:36].[CH3:29][O:28][CH2:27][C@H:10]1[CH2:9][NH:8][CH2:14][C:13]2[N:15]=[CH:16][C:17]([N:19]3[CH2:23][CH2:22][CH2:21][CH:20]3[CH2:24][O:25][CH3:26])=[N:18][C:12]=2[O:11]1参加物
5
反応物 2
生成物 1
試薬・触媒・溶媒 2
反応条件
- 温度
- 50 °C
実験手順
To a solution of (6R)-8-benzyl-6-(methoxymethyl)-3-[2-(methoxymethyl)pyrrolidin-1-yl]-6,7,8,9-tetrahydropyrazino[2,3-f][1,4]oxazepine (329 mg) in methanol (10 mL) was added 20% Pd(OH)2/C (40 mg), and the mixture was stirred under a hydrogen atmosphere at 50° C. for 3 hr. The reaction mixture was filtered, and the filtrate was concentrated under reduced pressure. To a solution of the obtained crude product in ethyl acetate (10 mL) was added a 4 N hydrogen chloride-ethyl acetate solution (227 μL), and the mixture was stirred for 30 min. The reaction mixture was filtered, and the obtained crystals were washed with ethyl acetate to give the title compound (155 mg, 54%).
後処理
- filtrationThe reaction mixture was filtered
- concentrationthe filtrate was concentrated under reduced pressure
- customTo a solution of the obtained crude product in ethyl acetate (10 mL)
- stirringthe mixture was stirred for 30 min
- filtrationThe reaction mixture was filtered
- washthe obtained crystals were washed with ethyl acetate
出典と根拠
- ORDレコード
- ord-622811282af1414eb77eb6acdfd1d638
- 出典データセット
- uspto-grants-2012_12
- 特許番号
- US08324201B2
反応ノート
読み込み中…