Water → 3-Amino-5-nitroindazole

HRID 227694

반응식

HRID 227694 반응식
[OH2:1].[NH2:2][NH2:3].Cl[C:5]1[CH:12]=[CH:11][C:10]([N+:13]([O-])=O)=[CH:9][C:6]=1[C:7]#[N:8].[OH2:16]>N1C=CC=CC=1>[N+:13]([C:10]1[CH:9]=[C:6]2[C:5](=[CH:12][CH:11]=1)[NH:3][N:2]=[C:7]2[NH2:8])([O-:16])=[O:1]

참가 물질

5

반응물 3

HCID 962WaterHCID 24654Hydrazine hydrate (1:1)HCID 855042-Chloro-5-nitrobenzonitrile

생성물 1

HCID 31366553-Amino-5-nitroindazole수율 80%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

Hydrazine monohydrate (2.1 mL, 44 mmol) was added to a solution of 2-chloro-5-nitrobenzonitrile (7.30 g, 40 mmol) in pyridine (30 mL) and the mixture was heated to reflux overnight. The dark red solution was then cooled, poured into H2O and the resulting solid filtered and dried to give the title compound as a dark red powder (5.7 g, 80%). NMR 1H NMR (400 MHz, DMSO-D6) δ ppm 8.95 (d, J=2.0, 1H), 8.06 (dd, J=9.2, 2.0, 1H), 7.34 (d, J=9.2, 1H), 5.98 (br s, 2H) MS m/z 179.0 [M+H]+

후처리

  1. temperaturethe mixture was heated
  2. temperatureto reflux overnight
  3. temperatureThe dark red solution was then cooled
  4. filtrationthe resulting solid filtered
  5. customdried

출처 및 근거

ORD 기록
ord-d4f7d523609746209c9ba165007cd546
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07560467B2

연결된 노트

불러오는 중…