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

HRID 81932ノート

反応式

HRID 81932 の反応式
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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1c273022fbee4b17b9446102647a86bb
出典データセット
uspto-grants-2014_09
特許番号
US08846710B2

反応ノート

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