Cesium carbonate → 6-(4-chlorophenyl)-3-{3-methoxy-4-[(1-methyl-3-piperidinyl)methoxy]phenyl}thieno[3,2-d]pyrimidin-4(3H)-one

HRID 1181367노트

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HRID 1181367 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[S:16][C:15]3[C:14](=[O:17])[N:13]([C:18]4[CH:23]=[CH:22][C:21]([OH:24])=[C:20]([O:25][CH3:26])[CH:19]=4)[CH:12]=[N:11][C:10]=3[CH:9]=2)=[CH:4][CH:3]=1.Cl[CH2:28][CH:29]1[CH2:34][CH2:33][CH2:32][N:31]([CH3:35])[CH2:30]1.C([O-])([O-])=O.[Cs+].[Cs+]>ClCCl>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[S:16][C:15]3[C:14](=[O:17])[N:13]([C:18]4[CH:23]=[CH:22][C:21]([O:24][CH2:28][CH:29]5[CH2:34][CH2:33][CH2:32][N:31]([CH3:35])[CH2:30]5)=[C:20]([O:25][CH3:26])[CH:19]=4)[CH:12]=[N:11][C:10]=3[CH:9]=2)=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 10796Cesium carbonateHCID 1036743-(Chloromethyl)-1-methylpiperidineHCID 589808956-(4-chlorophenyl)-3-(4-hydroxy-3-methoxyphenyl)thieno[3,2-d]pyrimidin-4(3H)-one

생성물 1

HCID 589808356-(4-chlorophenyl)-3-{3-methoxy-4-[(1-methyl-3-piperidinyl)methoxy]phenyl}thieno[3,2-d]pyrimidin-4(3H)-one

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution containing 6-(4-chlorophenyl)-3-(4-hydroxy-3-methoxyphenyl)thieno[3,2-d]pyrimidin-4(3H)-one (77 mg, 0.20 mmol, the preparation of which may be found in Example K1) and 3-(chloromethyl)-1-methylpiperidine (74 mg) was mixed with Cs2CO3 (261 mg, 0.80 mmol) and the resultant mixture was heated at 85° C. for 3 hours. The mixture was then cooled to room temperature, diluted with dichlormethane, washed with a saturated solution of NaHCO3 and brine, dried (MgSO4), and concentrated under reduced pressure. The resultant residue was purified by column chromatography to provide the title compound.

후처리

  1. customthe preparation of which
  2. washwashed with a saturated solution of NaHCO3 and brine
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated under reduced pressure
  5. customThe resultant residue was purified by column chromatography

출처 및 근거

ORD 기록
ord-e7f9ea7ad6e842f5a3167c33f34df315
출처 데이터셋
uspto-grants-2007_10
특허 번호
US07285557B2

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