Triethylamine → 5-Benzyluracil

HRID 1975488ノート

反応式

HRID 1975488 の反応式
[CH2:1]([C:8]1[C:9](=[O:20])[NH:10][C:11](=[O:19])[NH:12][C:13]=1OS(C)(=O)=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CCN(CC)CC.[OH-].[Na+]>CO.[Pd]>[CH2:1]([C:8]1[C:9](=[O:20])[NH:10][C:11](=[O:19])[NH:12][CH:13]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

6

反応物 3

HCID 8471TriethylamineHCID 14798Sodium HydroxideHCID 11141002HCID 11141002、化合物

生成物 1

HCID 2362125-Benzyluracil収率 79.8%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

A solution of 5-benzyl-6-methanesulphonyloxy-2,4-(1H,3H)-pyrimidinedione (3 g) and Et3N (2.1 ml) in MeOH was hydrogenated in the presence of Pd/C 5% (0.3 g) for 3 hr at 35° C. NaOH 5% (2.5 eq) was added and the catalyst filtered off. The solution was acidified to pH 2 with HCl 10%. The precipitated white solid was then collected by filtration, washed with water, ether and dried under vacuum to yield the desired 5-benzyl-2,4-(1H,3H)-pyrimidinedione: 1.635 g, 79.8% yield.

後処理

  1. filtrationthe catalyst filtered off
  2. filtrationThe precipitated white solid was then collected by filtration
  3. washwashed with water, ether
  4. customdried under vacuum

出典と根拠

ORDレコード
ord-a1c6c60505fc4ebcb2e1361cee514383
出典データセット
uspto-grants-1994_02
特許番号
US05286861

反応ノート

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