Sodium Bicarbonate → 2-{4-[(Naphthalen-2-yl)methyl]piperazin-1-yl}pyrimidin-5-ol

HRID 1288567ノート

反応式

HRID 1288567 の反応式
[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[CH2:11][N:12]1[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1.Cl[C:19]1[N:24]=[CH:23][C:22]([OH:25])=[CH:21][N:20]=1.C(=O)(O)[O-].[Na+]>CN(C)C=O>[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[CH2:11][N:12]1[CH2:13][CH2:14][N:15]([C:19]2[N:24]=[CH:23][C:22]([OH:25])=[CH:21][N:20]=2)[CH2:16][CH2:17]1

参加物

5

反応物 3

HCID 516892Sodium BicarbonateHCID 9105371-(Naphthalen-2-ylmethyl)piperazineHCID 145957002-Chloro-5-pyrimidinol

生成物 1

HCID 215029112-{4-[(Naphthalen-2-yl)methyl]piperazin-1-yl}pyrimidin-5-ol

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a mixture of 4.50 g. of 1-(β-napthylmethyl)piperazine(as prepared in Example 7), 2.5 g. of 2-chloro-5-hydroxypyrimidine in 30 ml. of dimethylformamide is added 2.0 g. of sodium bicarbonate and the mixture is refluxed for six hours. The mixture is cooled and filtered and the filtrate concentrated to a small volume in vacuo. The concentrate is diluted with 100 ml. of water and the insoluble material is washed with water and hexane to yield 1-(β-napthylmethyl)-4-(5-hydroxy-2-pyrimidinyl)piperazine.

後処理

  1. additionTo a mixture of 4.50 g
  2. temperatureThe mixture is cooled
  3. filtrationfiltered
  4. concentrationthe filtrate concentrated to a small volume in vacuo
  5. additionThe concentrate is diluted with 100 ml
  6. washof water and the insoluble material is washed with water and hexane

出典と根拠

ORDレコード
ord-bb1802a043204db3a429850a29a37f65
出典データセット
uspto-grants-1976_10
特許番号
US03988457

反応ノート

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