1,3-Dimethyl-6-hydroxylaminouracil → Isoxazolo(3,4-d)pyrimidine-4,6(5H,7H)-dione, 5,7-dimethyl-

HRID 65915ノート

反応式

HRID 65915 の反応式
[CH3:1][N:2]1[C:9]([NH:10][OH:11])=[CH:8][C:6](=[O:7])[N:5]([CH3:12])[C:3]1=[O:4].[CH:13]([O-])([O-])OCC>CN(C)C=O>[CH3:12][N:5]1[C:6](=[O:7])[C:8]2=[CH:13][O:11][N:10]=[C:9]2[N:2]([CH3:1])[C:3]1=[O:4]

参加物

4

反応物 2

HCID 27859331,3-Dimethyl-6-hydroxylaminouracilHCID 53630039Ethylorthoformate

生成物 1

HCID 2785556Isoxazolo(3,4-d)pyrimidine-4,6(5H,7H)-dione, 5,7-dimethyl-

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 2 g of 1,3-dimethyl-6-hydroxyaminouracil, 20 ml of dimethylformamide and 20 ml of ethyl orthoformate is boiled at 160° C. for 1 hour, after which the solvent is distilled off. To the residue is added ethanol and the resultant crystals are collected by filtration. As recrystallized from hot water, 1.0 g of the captioned compound is obtained as colorless prisms, melting point: 170°-171° C.

後処理

  1. customfor 1 hour
  2. distillationafter which the solvent is distilled off
  3. additionTo the residue is added ethanol
  4. filtrationthe resultant crystals are collected by filtration
  5. customAs recrystallized from hot water

出典と根拠

ORDレコード
ord-236fd08383f64e2cb363e09d99783ced
出典データセット
uspto-grants-1978_12
特許番号
US04129654

反応ノート

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