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

HRID 2197519노트

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HRID 2197519 반응식
[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

참가 물질

6

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온도
80 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-eb4408e076ff470ba82ccfd12655de0d
출처 데이터셋
uspto-grants-2012_12
특허 번호
US08338594B2

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