HCID 70004538、化合物 → HCID 70003854、化合物

HRID 580900ノート

反応式

HRID 580900 の反応式
[OH:1][CH2:2][CH2:3][C:4]1[C:9](=[O:10])[N:8]2[CH:11]=[CH:12][CH:13]=[C:14]([O:15][CH3:16])[C:7]2=[N:6][C:5]=1[CH3:17].[H][H]>CO.[Pd]>[OH:1][CH2:2][CH2:3][C:4]1[C:9](=[O:10])[N:8]2[CH2:11][CH2:12][CH2:13][CH:14]([O:15][CH3:16])[C:7]2=[N:6][C:5]=1[CH3:17]

参加物

5

反応物 2

HCID 70004538HCID 70004538、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 70003854HCID 70003854、化合物収率 71%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

A mixture of intermediate 10 (14 g) in methanol (250 ml) was hydrogenated at 50° C. with palladium on activated carbon (10%) (2 g) as a catalyst. After uptake of hydrogen (2 eq.), the catalyst was filtered off. The filtrate was evaporated and the residue was purified by column chromatography over silica gel (eluent: CH2Cl2 /CH3OH 95/5). The pure fractions were collected and the solvent was evaporated, yielding 10 g (71%) of (±)-6,7,8,9-tetrahydro-3-(2-hydroxyethyl)-9-methoxy-2-methyl-4H-pyrido[1,2-a]-pyrimidin-4-one (intermediate 11).

後処理

  1. customThe filtrate was evaporated
  2. customthe residue was purified by column chromatography over silica gel (eluent: CH2Cl2 /CH3OH 95/5)
  3. customThe pure fractions were collected
  4. customthe solvent was evaporated

出典と根拠

ORDレコード
ord-8f108b0d82d044378763685264b997cb
出典データセット
uspto-grants-1999_07
特許番号
US05919788

反応ノート

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