Sodium Carbonate → 2-(4-Naphthalen-2-ylmethyl-piperazin-1-yl)-pyrimidine

HRID 1288563

반응식

HRID 1288563 반응식
Cl[CH2:2][C:3]1[CH:12]=[CH:11][C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=1.C(=O)([O-])[O-].[Na+].[Na+].[N:19]1[CH:24]=[CH:23][CH:22]=[N:21][C:20]=1[N:25]1[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]1>CN(C)C=O>[CH:4]1[C:5]2[C:10](=[CH:9][CH:8]=[CH:7][CH:6]=2)[CH:11]=[CH:12][C:3]=1[CH2:2][N:28]1[CH2:29][CH2:30][N:25]([C:20]2[N:19]=[CH:24][CH:23]=[CH:22][N:21]=2)[CH2:26][CH2:27]1

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 756322-(Chloromethyl)naphthaleneHCID 887471-(2-Pyrimidinyl)piperazine

생성물 1

HCID 7509752-(4-Naphthalen-2-ylmethyl-piperazin-1-yl)-pyrimidine

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a mixture containing 5.0 g. of β-chloromethylnaphthalene, 3.0 g. of sodium carbonate and 30 ml. of dimethylformamide is added 4.6 g. of pyrimidinylpiperazine. The mixture is stirred and heated on a steam bath for approximately two hours. The mixture is then cooled, filtered and the filtrate is concentrated to a small volume in vacuo. The residue is washed with water and crystallized from ethanol to yield 1-(β-napthylmethyl)-4-(2-pyrimidinyl)-piperazine having a melting point of 109°-110° C.

후처리

  1. additionTo a mixture containing 5.0 g
  2. temperatureheated on a steam bath for approximately two hours
  3. temperatureThe mixture is then cooled
  4. filtrationfiltered
  5. concentrationthe filtrate is concentrated to a small volume in vacuo
  6. washThe residue is washed with water
  7. customcrystallized from ethanol

출처 및 근거

ORD 기록
ord-c5dac7cbb61a44458ac7acc3ae0d156c
출처 데이터셋
uspto-grants-1976_10
특허 번호
US03988457

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