Hydrochloric Acid → 4-Amino-5-(4-nitrophenyl)pyrrolo[2,1-f][1,2,4]triazine-6-carboxylic acid

HRID 2197519ノート

反応式

HRID 2197519 の反応式
[NH2:1][C:2]1[C:7]2=[C:8]([C:16]3[CH:21]=[CH:20][C:19]([N+:22]([O-:24])=[O:23])=[CH:18][CH:17]=3)[C:9]([C:11]([O:13]CC)=[O:12])=[CH:10][N:6]2[N:5]=[CH:4][N:3]=1.[OH-].[Na+].Cl>C(O)C.C1COCC1>[NH2:1][C:2]1[C:7]2=[C:8]([C:16]3[CH:17]=[CH:18][C:19]([N+:22]([O-:24])=[O:23])=[CH:20][CH:21]=3)[C:9]([C:11]([OH:13])=[O:12])=[CH:10][N:6]2[N:5]=[CH:4][N:3]=1

参加物

6

反応条件

温度
80 °C

実験手順

A suspension of ethyl 4-amino-5-(4-nitrophenyl)pyrrolo[2,1-f][1,2,4]triazine-6-carboxylate (1.04 g, 3.18 mmol) in ethanol (10 mL), THF (5 mL) and 1N aqueous sodium hydroxide solution (5.56 mL, 5.56 mmol) was heated (80° C.) for 6 h. The homogeneous solution was cooled to rt and treated dropwise with 1N hydrochoric acid (5.56 mL). The reaction was concentrated in vacuo and the resulting solid triturated with water to give the desired product in quantitative yield. This material could be used without further purification. ES-MS 300.2 (MH)+; HPLC RT (Method A) 1.37 min.

後処理

  1. temperatureThe homogeneous solution was cooled to rt
  2. concentrationThe reaction was concentrated in vacuo
  3. customthe resulting solid triturated with water

出典と根拠

ORDレコード
ord-eb4408e076ff470ba82ccfd12655de0d
出典データセット
uspto-grants-2012_12
特許番号
US08338594B2

反応ノート

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