Water → N-(2-fluoro-2-methylpropyl)-3-nitro[1,5]naphthyridin-4-amine

HRID 81932노트

반응식

HRID 81932 반응식
Cl.[F:2][C:3]([CH3:7])([CH3:6])[CH2:4][NH2:5].C(N(CC)CC)C.Cl[C:16]1[C:25]2[C:20](=[CH:21][CH:22]=[CH:23][N:24]=2)[N:19]=[CH:18][C:17]=1[N+:26]([O-:28])=[O:27].O>C(Cl)Cl>[F:2][C:3]([CH3:7])([CH3:6])[CH2:4][NH:5][C:16]1[C:25]2[C:20](=[CH:21][CH:22]=[CH:23][N:24]=2)[N:19]=[CH:18][C:17]=1[N+:26]([O-:28])=[O:27]

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 131227874-Chloro-3-nitro-1,5-naphthyridineHCID 552896302-Fluoro-2-methylpropan-1-amine hydrochloride

생성물 1

HCID 68934906N-(2-fluoro-2-methylpropyl)-3-nitro[1,5]naphthyridin-4-amine수율 100.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

2-Fluoro-2-methylpropan-1-amine hydrochloride (4.02 g, 31.4 mmol) was dissolved in 80 mL of dry CH2Cl2. Triethylamine (13.1 mL, 94.2 mmol) and 4-chloro-3-nitro[1,5]naphthyridine (6.56 g, 31.4 mmol) were then added and the reaction was stirred under N2 for 2 days. The reaction mixture was then concentrated under reduced pressure to give a dark-yellow solid. The solid was treated with 200 mL of H2O and the mixture was heated to reflux with rapid stirring. The mixture was cooled and the yellow solid was isolated by filtration. The material was washed with H2O and the dried under vacuum to give N-(2-fluoro-2-methylpropyl)-3-nitro[1,5]naphthyridin-4-amine (8.36 g) as a yellow powder.

후처리

  1. concentrationThe reaction mixture was then concentrated under reduced pressure
  2. customto give a dark-yellow solid
  3. temperaturethe mixture was heated
  4. temperatureto reflux with rapid stirring
  5. temperatureThe mixture was cooled
  6. customthe yellow solid was isolated by filtration
  7. washThe material was washed with H2O
  8. customthe dried under vacuum

출처 및 근거

ORD 기록
ord-1c273022fbee4b17b9446102647a86bb
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846710B2

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