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

HRID 598012ノート

反応式

HRID 598012 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 warm to room temperature slowly and stirred overnight. The solvent was removed under reduced pressure, and the solid residue was mixed with deionized water (200 mL). The solid was isolated by filtration, washed with deionized 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 warm to room temperature slowly
  4. customThe solvent was removed under reduced pressure
  5. additionthe solid residue was mixed with deionized water (200 mL)
  6. customThe solid was isolated by filtration
  7. washwashed with deionized 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-2b0a54ca758d4c879e2b723ceea13125
出典データセット
uspto-grants-2011_03
特許番号
US07897609B2

反応ノート

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