Potassium Carbonate → 3,5-Dimethyl-2-[4-[4-(2-piperidinoethoxy)benzoyl]-benzylthio]thieno[2,3-d]pyrimidin-4(3H)-one hydrochloride

HRID 1291350노트

반응식

HRID 1291350 반응식
[CH3:1][N:2]1[C:7](=[O:8])[C:6]2[C:9]([CH3:12])=[CH:10][S:11][C:5]=2[N:4]=[C:3]1[S:13][CH2:14][C:15]1[CH:20]=[CH:19][C:18]([C:21](=[O:29])[C:22]2[CH:27]=[CH:26][C:25]([OH:28])=[CH:24][CH:23]=2)=[CH:17][CH:16]=1.Cl.[Cl:31][CH2:32][CH2:33][N:34]1[CH2:39][CH2:38][CH2:37][CH2:36][CH2:35]1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[ClH:31].[CH3:1][N:2]1[C:7](=[O:8])[C:6]2[C:9]([CH3:12])=[CH:10][S:11][C:5]=2[N:4]=[C:3]1[S:13][CH2:14][C:15]1[CH:16]=[CH:17][C:18]([C:21](=[O:29])[C:22]2[CH:23]=[CH:24][C:25]([O:28][CH2:32][CH2:33][N:34]3[CH2:39][CH2:38][CH2:37][CH2:36][CH2:35]3)=[CH:26][CH:27]=2)=[CH:19][CH:20]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 74826Piperidine, 1-(2-chloroethyl)-, hydrochlorideHCID 189188093,5-dimethyl-2-[4-(4-hydroxybenzoyl)benzylthio]thieno[2,3-d]pyrimidin-4(3H)-one

생성물 1

HCID 189191603,5-Dimethyl-2-[4-[4-(2-piperidinoethoxy)benzoyl]-benzylthio]thieno[2,3-d]pyrimidin-4(3H)-one hydrochloride수율 77.9%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of 3,5-dimethyl-2-[4-(4-hydroxybenzoyl)benzylthio]thieno[2,3-d]pyrimidin-4(3H)-one (255 mg), 1-(2-chloroethyl)piperidine hydrochloride (122 mg) and potassium carbonate (250 mg) in DMF (8 ml) was stirred at 60° C. for 15 hours. This reaction mixture was concentrated, the residue was dissolved in ethyl acetate, and the solution was washed with water and dried. Then, HCl/ethyl acetate was added and the precipitated hydrochloride was collected by filtration and dried to provide the title compound as colorless solid (268 mg).

후처리

  1. concentrationThis reaction mixture was concentrated
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washthe solution was washed with water
  4. customdried
  5. additionThen, HCl/ethyl acetate was added
  6. filtrationthe precipitated hydrochloride was collected by filtration
  7. customdried

출처 및 근거

ORD 기록
ord-94b64c856fe94438baf8da1b00e709ec
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05753664

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