Acetic Acid → 3-methyl-5,6,7,8-tetrahydro-1H-pyrido[4,3-d]pyrimidine-2,4-dione

HRID 742961

반응식

HRID 742961 반응식
C([N:8]1[CH2:20][CH2:19][C:11]2[NH:12][C:13](=[O:18])[N:14]([CH3:17])[C:15](=[O:16])[C:10]=2[CH2:9]1)C1C=CC=CC=1.C(O)(=O)C>O.[Pd]>[CH3:17][N:14]1[C:15](=[O:16])[C:10]2[CH2:9][NH:8][CH2:20][CH2:19][C:11]=2[NH:12][C:13]1=[O:18]

참가 물질

5

반응물 2

HCID 176Acetic AcidHCID 100160286-benzyl-3-methyl-5,6,7,8-tetrahydro-1H-pyrido[4,3-d]pyrimidine-2,4-dione

생성물 1

HCID 102414233-methyl-5,6,7,8-tetrahydro-1H-pyrido[4,3-d]pyrimidine-2,4-dione수율 179.8%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 962Water용매

실험 절차

A solution of 96 g of 6-benzyl-3-methyl-5,6,7,8-tetra-hydro-1H-pyrido[4,3-d]pyrimidine-2,4-dione from c) in 1.5 1 of glacial acetic acid was debenzylated by hydrogenolysis for 6 h on 14.6 g of 10% palladium/activated charcoal at 25° C. and 3.5 bar. After the catalyst had been filtered off, the filtrate was concentrated under reduced pressure. The above preparation was repeated. The two crude products were combined, dissolved in water and precipitated, with stirring, by the addition of 33% sodium hydroxide solution to pH 6.9. The precipitate was washed with water and dried at 60° C. under reduced pressure to give 115.3 g of 3-methyl-5,6,7,8-tetrahydro-1H-pyrido[4,3-d]pyrimidine-2,4-dione.

후처리

  1. filtrationAfter the catalyst had been filtered off
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customThe above preparation
  4. customprecipitated
  5. washThe precipitate was washed with water
  6. customdried at 60° C. under reduced pressure

출처 및 근거

ORD 기록
ord-9554e01e27824ec083075b202565eeed
출처 데이터셋
uspto-grants-1996_09
특허 번호
US05556854

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