Diethyl 2-(p-tolyl)malonate → 5-(4-Methylphenyl)-4,6-dihydroxy-2-n-propylpyrimidine

HRID 2317ノート

反応式

HRID 2317 の反応式
C(O[C:4](=[O:18])[CH:5]([C:11]1[CH:16]=[CH:15][C:14]([CH3:17])=[CH:13][CH:12]=1)[C:6]([O:8]CC)=O)C.Cl.[C:20]([NH2:25])(=[NH:24])[CH2:21][CH2:22][CH3:23].C[O-].[Na+]>CO>[CH3:17][C:14]1[CH:13]=[CH:12][C:11]([C:5]2[C:4]([OH:18])=[N:24][C:20]([CH2:21][CH2:22][CH3:23])=[N:25][C:6]=2[OH:8])=[CH:16][CH:15]=1

参加物

5

反応物 3

HCID 570878Diethyl 2-(p-tolyl)malonateHCID 10942334Sodium MethoxideHCID 12828983Butanimidamide hydrochloride

生成物 1

HCID 1784184665-(4-Methylphenyl)-4,6-dihydroxy-2-n-propylpyrimidine収率 56.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of diethyl(4-methylphenyl)malonate (9.45 g) and butyramidine hydrochloride (5.00 g) in methanol (25 ml) is added 28% sodium methoxide (19.67 g) under ice-cooling, and the mixture is stirred at room temperature overnight. After the reaction is complete, the reaction solution is concentrated to the half volume thereof, and the resultant is diluted with water. The mixture is acidified with 10% hydrochloric acid, and the precipitated crystals are collected by filtration, washed, and dried to give 5-(4-methylphenyl)-4,6-dihydroxy-2-n-propylpyrimidine (5.17 g) as crystalline powder.

後処理

  1. temperaturecooling
  2. concentrationthe reaction solution is concentrated to the half volume
  3. additionthe resultant is diluted with water
  4. filtrationthe precipitated crystals are collected by filtration
  5. washwashed
  6. customdried

出典と根拠

ORDレコード
ord-fcdab10bc84144e59957a7d86566aed7
出典データセット
uspto-grants-1998_03
特許番号
US05728706

反応ノート

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