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

HRID 909359노트

반응식

HRID 909359 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
10 °C

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-0233111dea2f40cb9799301eb806888f
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08017779B2

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