1-((4R)-2,2-dimethyl-1,3-dioxolan-4-yl)methanamine → HCID 68817756、化合物

HRID 9483ノート

反応式

HRID 9483 の反応式
[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

反応物 2

HCID 101540731-((4R)-2,2-dimethyl-1,3-dioxolan-4-yl)methanamineHCID 219843617-Bromo-4-chloro-3-nitroquinoline

生成物 1

HCID 68817756HCID 68817756、化合物収率 88.4%

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

  1. customThe crude product was triturated with water (200 mL)
  2. customisolated by filtration
  3. washwashed with water
  4. customdried
  5. customThe suspension was sonicated
  6. customthe resulting solid was isolated by filtration
  7. customdried for four hours in a vacuum oven at 40° C.

出典と根拠

ORDレコード
ord-6ce4ecf087dd4b5e9dfdb947815f2d30
出典データセット
uspto-grants-2006_08
特許番号
US07091214B2

反応ノート

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