1-((4R)-2,2-dimethyl-1,3-dioxolan-4-yl)methanamine → HCID 68817756、化合物
反応式
[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6](Cl)=[C:7]([N+:12]([O-:14])=[O:13])[CH:8]=[N:9]2)=[CH:4][CH:3]=1.[CH3:16][C:17]1([CH3:24])[O:21][C@H:20]([CH2:22][NH2:23])[CH2:19][O:18]1>>[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6]([NH:23][CH2:22][C@@H:20]3[CH2:19][O:18][C:17]([CH3:24])([CH3:16])[O:21]3)=[C:7]([N+:12]([O-:14])=[O:13])[CH:8]=[N:9]2)=[CH:4][CH:3]=1参加物
3
実験手順
7-Bromo-4-chloro-3-nitroquinoline (22.00 g, 76.52 mmol) was treated with (R)-2,2-dimethyl-1,3-dioxolane-4-methanamine (11.61 g, 114.8 mmol) according to the method described in Part A of Examples 152-156. The crude product was triturated with water (200 mL), isolated by filtration, washed with water, dried, and suspended in diethyl ether (100 mL). The suspension was sonicated, and the resulting solid was isolated by filtration, and dried for four hours in a vacuum oven at 40° C. to provide 25.84 g of (R)-(7-bromo-3-nitroquinolin-4-yl)-(2,2-dimethyl-1,3-dioxolan-4-ylmethyl)amine as a yellow solid, mp 136-137° C.
後処理
- customThe crude product was triturated with water (200 mL)
- customisolated by filtration
- washwashed with water
- customdried
- customThe suspension was sonicated
- customthe resulting solid was isolated by filtration
- customdried for four hours in a vacuum oven at 40° C.
出典と根拠
- ORDレコード
- ord-a15677d782e34ec881f196d5673e90c7
- 出典データセット
- uspto-grants-2009_10
- 特許番号
- US07598382B2
反応ノート
読み込み中…