2-Propanol, 1-amino-2-methyl- → 1-[(7-Bromo-3-nitro[1,5]naphthyridin-4-yl)amino]-2-methylpropan-2-ol

HRID 909359ノート

反応式

HRID 909359 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)=[N:4][CH:3]=1.[NH2:16][CH2:17][C:18]([CH3:21])([OH:20])[CH3:19]>ClCCl>[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6]([NH:16][CH2:17][C:18]([CH3:21])([OH:20])[CH3:19])=[C:7]([N+:12]([O-:14])=[O:13])[CH:8]=[N:9]2)=[N:4][CH:3]=1

参加物

4

反応物 2

HCID 951022-Propanol, 1-amino-2-methyl-HCID 574578377-Bromo-4-chloro-3-nitro[1,5]naphthyridine

生成物 1

HCID 670524611-[(7-Bromo-3-nitro[1,5]naphthyridin-4-yl)amino]-2-methylpropan-2-ol

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
10 °C

実験手順

A mixture of 7-bromo-4-chloro-3-nitro[1,5]naphthyridine (92.5 g, 321 mmol) and dichloromethane (1.5 L) was cooled to 10° C. 1-Amino-2-methylpropan-2-ol (63.01 g, 707 mmol) was added dropwise over a period of 30 minutes; during the addition, the reaction temperature did not rise above 13° C. The reaction mixture was allowed to slowly warm to room temperature and stirred overnight. The solvent was removed under reduced pressure, and the solid residue was mixed with water (200 mL). The solid was isolated by filtration, washed with water (2×200 mL), and dried in a vacuum oven overnight at 35° C. to provide 1-[(7-bromo-3-nitro[1,5]naphthyridin-4-yl)amino]-2-methylpropan-2-ol.

後処理

  1. additionduring the addition
  2. customdid not rise above 13° C
  3. temperatureto slowly warm to room temperature
  4. customThe solvent was removed under reduced pressure
  5. additionthe solid residue was mixed with water (200 mL)
  6. customThe solid was isolated by filtration
  7. washwashed with water (2×200 mL)
  8. customdried in a vacuum oven overnight at 35° C.

出典と根拠

ORDレコード
ord-0233111dea2f40cb9799301eb806888f
出典データセット
uspto-grants-2011_09
特許番号
US08017779B2

反応ノート

読み込み中…