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

HRID 742961

反応式

HRID 742961 の反応式
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]

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9554e01e27824ec083075b202565eeed
出典データセット
uspto-grants-1996_09
特許番号
US05556854

関連ノート

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