Nitric Acid → 2-(2-Propoxy-5-nitrophenyl)purin-6-one

HRID 1460972ノート

反応式

HRID 1460972 の反応式
[N+:1]([O-:4])(O)=[O:2].[CH2:5]([O:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[C:15]1[N:23]=[C:22]2[C:18](=[N:19][CH:20]=[N:21]2)[C:17](=[O:24])[N:16]=1)[CH2:6][CH3:7].[OH-].[NH4+]>S(=O)(=O)(O)O>[CH2:5]([O:8][C:9]1[CH:14]=[CH:13][C:12]([N+:1]([O-:4])=[O:2])=[CH:11][C:10]=1[C:15]1[N:23]=[C:22]2[C:18](=[N:19][CH:20]=[N:21]2)[C:17](=[O:24])[N:16]=1)[CH2:6][CH3:7]

参加物

5

反応物 3

HCID 944Nitric AcidHCID 14923Ammonium HydroxideHCID 18409955HCID 18409955、化合物

生成物 1

HCID 212508282-(2-Propoxy-5-nitrophenyl)purin-6-one

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒2 回

実験手順

A mixture of fuming nitric acid (0.23 ml) and sulphuric acid (4 ml) was added dropwise to a stirred solution of 2-(2-propoxyphenyl)purin-6-one (1.0 g) in sulphuric acid (4 ml) at 0° to -5° C. The temperature was maintained between -5° C. and +4° C. for 20 hours and then the mixture was poured into ice-water. The filtered solution was treated with concentrated ammonium hydroxide to pH 9 to give a crude product, 0.55 g. Recrystallisation twice from aqueous ethanol then once from acetonitrile gave the title compound, 0.2 g, m.p. 254°-256° C.

後処理

  1. temperatureThe temperature was maintained between -5° C. and +4° C. for 20 hours
  2. customto give a crude product, 0.55 g
  3. customRecrystallisation twice from aqueous ethanol

出典と根拠

ORDレコード
ord-87c56d5302564a408b8e66e7bb46ef52
出典データセット
uspto-grants-1991_12
特許番号
US05073559

反応ノート

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