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

HRID 65915노트

반응식

HRID 65915 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-236fd08383f64e2cb363e09d99783ced
출처 데이터셋
uspto-grants-1978_12
특허 번호
US04129654

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