O-(2,4-dinitrophenyl)hydroxylamine → 1-Amino-4-((tert-butoxycarbonyl)amino)-3-fluoropyridin-1-ium 2,4-dinitrophenolate

HRID 1476753ノート

反応式

HRID 1476753 の反応式
[F:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1[NH:8][C:9](=[O:15])[O:10][C:11]([CH3:14])([CH3:13])[CH3:12].[N+:16]([C:19]1[CH:24]=[C:23]([N+:25]([O-:27])=[O:26])[CH:22]=[CH:21][C:20]=1[O:28]N)([O-:18])=[O:17]>CC#N>[NH2:16][N+:4]1[CH:5]=[CH:6][C:7]([NH:8][C:9]([O:10][C:11]([CH3:12])([CH3:14])[CH3:13])=[O:15])=[C:2]([F:1])[CH:3]=1.[N+:16]([C:19]1[CH:24]=[C:23]([N+:25]([O-:27])=[O:26])[CH:22]=[CH:21][C:20]=1[O-:28])([O-:18])=[O:17]

参加物

4

反応物 2

HCID 87140O-(2,4-dinitrophenyl)hydroxylamineHCID 71748416tert-Butyl (3-fluoropyridin-4-yl)carbamate

生成物 1

HCID 896190191-Amino-4-((tert-butoxycarbonyl)amino)-3-fluoropyridin-1-ium 2,4-dinitrophenolate

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒2 回

反応条件

温度
40 °C

実験手順

A solution of tert-butyl (3-fluoropyridin-4-yl)carbamate (25.0 g, 125 mmol) in MeCN (200 ml), was added O-(2,4-dinitrophenyl)hydroxylamine (26.64 g, 125 mmol) in MeCN (200 ml), drop wise over 30 min at RT, reaction mass was stirred at 40° C. for 12 hrs, reaction mass was concentrated at temperature below 40° C. under reduced pressure to afford Int-11 (50 g) which was used in the next step without further purification.

後処理

  1. customreaction mass
  2. customreaction mass
  3. concentrationwas concentrated at temperature below 40° C. under reduced pressure
  4. customto afford Int-11 (50 g) which
  5. customwas used in the next step without further purification

出典と根拠

ORDレコード
ord-56f9c4daa91c44b3b68ba6cd366eaa65
出典データセット
uspto-grants-2016_08
特許番号
US09402833B2

反応ノート

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