Acetic Acid → HCID 178481542, 화합물

HRID 2258473노트

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HRID 2258473 반응식
N[C:2]1[N:7]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[C:6](=[O:14])[N:5]([CH3:15])[C:4](=[O:16])[CH:3]=1.Cl.C(O)(=[O:20])C>>[OH:20][C:2]1[N:7]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[C:6](=[O:14])[N:5]([CH3:15])[C:4](=[O:16])[CH:3]=1

참가 물질

4

반응물 3

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 16492566-Amino-3-methyl-1-phenylpyrimidine-2,4(1H,3H)-dione

생성물 1

HCID 178481542HCID 178481542, 화합물수율 68%

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온도
100 °C

실험 절차

6-Amino-3-methyl-1-phenyluracil as obtained in Reference Example 1 (8.7 g, 40 mM) was dissolved in 80 ml of acetic acid and hydrochloric acid (16 ml) was added, followed by heating at 100° C. for 1 hour. The solvent acetic acid was then distilled off under reduced pressure and water war added to the residue. The pH of the resulting solution was adjusted to 1 by adding hydrochloric acid and a product was extracted with dichloromethane. After the solvent dichloromethane was distilled off under reduced pressure from the dichloromethane layer, crystallization with ethanol was performed to give 6-hydroxy-3-methyl-1-phenyluracil (yield: 5.9 g, or 68% based on 6-amino-3-methyl-1-phenyluracil).

후처리

  1. distillationThe solvent acetic acid was then distilled off under reduced pressure and water war
  2. additionadded to the residue
  3. additionby adding hydrochloric acid
  4. extractiona product was extracted with dichloromethane
  5. distillationAfter the solvent dichloromethane was distilled off under reduced pressure from the dichloromethane layer, crystallization with ethanol

출처 및 근거

ORD 기록
ord-05a1dbe9acbc41669f9f1ebfef38eac1
출처 데이터셋
uspto-grants-1997_08
특허 번호
US05661153

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