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

HRID 1288567노트

반응식

HRID 1288567 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-bb1802a043204db3a429850a29a37f65
출처 데이터셋
uspto-grants-1976_10
특허 번호
US03988457

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