Water → 3-Amino-5-nitroindazole

HRID 227694

反応式

HRID 227694 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 31366553-Amino-5-nitroindazole収率 80%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

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]+

後処理

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

出典と根拠

ORDレコード
ord-d4f7d523609746209c9ba165007cd546
出典データセット
uspto-grants-2009_07
特許番号
US07560467B2

関連ノート

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