Potassium Carbonate → HCID 50852345, 화합물

HRID 612412노트

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HRID 612412 반응식
[CH2:1]([O:3][C:4]([C:6]1[C:7]([N:12]2[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]2)=[N:8][CH:9]=[CH:10][CH:11]=1)=[O:5])[CH3:2].CS(O[CH2:23][CH2:24][CH:25]=[C:26]1[C:32]2[CH:33]=[CH:34][CH:35]=[CH:36][C:31]=2[CH2:30][CH2:29][C:28]2[CH:37]=[CH:38][CH:39]=[CH:40][C:27]1=2)(=O)=O.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[CH2:1]([O:3][C:4]([C:6]1[C:7]([N:12]2[CH2:13][CH2:14][N:15]([CH2:23][CH2:24][CH:25]=[C:26]3[C:27]4[CH:40]=[CH:39][CH:38]=[CH:37][C:28]=4[CH2:29][CH2:30][C:31]4[CH:36]=[CH:35][CH:34]=[CH:33][C:32]3=4)[CH2:16][CH2:17]2)=[N:8][CH:9]=[CH:10][CH:11]=1)=[O:5])[CH3:2]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 17127123-(10,11-dihydro-5H-dibenzo[a,d]cyclohepten-5-ylidene)propyl methanesulfonateHCID 11615598Ethyl 2-(piperazin-1-yl)nicotinate

생성물 1

HCID 50852345HCID 50852345, 화합물수율 48.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
60 °C

실험 절차

A mixture of 2-(1-piperazinyl)-3-pyridinecarboxylic acid ethyl ester (4.6 g, 0.019 mol), 3-(10,11-dihydro-5H-dibenzo[a,d]cyclohepten-5-ylidene)-1-propyl methanesulfonate (5.0 g, 0.015 mol) and potassium carbonate (4.8 g) in N,N-dimethylformamide (50 ml) was heated to 60° C. for 5 h. After standing overnight, the solid was filtered off and washed with benzene. The filtrate was diluted with benzene (200 ml) and washed with water (4×100 ml). The organic solution was dried (MgSO4) and the solvent evaporated in vacuo. The residue (7.8 g) was purified by column chromatography on silica gel using benzene and a benzene-ethyl acetate mixture as eluents, affording 2-(4-(3-(10,11-dihydro-5H-dibenzo[a,d]cyclohepten-5-ylidene)-1-propyl)-1-piperazinyl)-3-pyridinecarboxylic acid ethyl ester (3.4 g, 48%) as an oil.

후처리

  1. filtrationthe solid was filtered off
  2. washwashed with benzene
  3. additionThe filtrate was diluted with benzene (200 ml)
  4. washwashed with water (4×100 ml)
  5. dry with materialThe organic solution was dried (MgSO4)
  6. customthe solvent evaporated in vacuo
  7. customThe residue (7.8 g) was purified by column chromatography on silica gel

출처 및 근거

ORD 기록
ord-0ed105fc719f4a58814f49b074d71418
출처 데이터셋
uspto-grants-1999_12
특허 번호
US06004961

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