Potassium Carbonate → 1-(6-chloropyrimidin-4-yl)-trans-2,6-dimethylhexahydro-1H-azepine

HRID 14574

반응식

HRID 14574 반응식
Cl[C:2]1[CH:7]=[C:6]([Cl:8])[N:5]=[CH:4][N:3]=1.C(=O)([O-])[O-].[K+].[K+].Cl.[CH3:16][C@H:17]1[CH2:23][CH2:22][CH2:21][C@H:20]([CH3:24])[CH2:19][NH:18]1.[Cl-].[NH4+]>C(#N)C>[Cl:8][C:6]1[N:5]=[CH:4][N:3]=[C:2]([N:18]2[CH2:19][C@@H:20]([CH3:24])[CH2:21][CH2:22][CH2:23][C@@H:17]2[CH3:16])[CH:7]=1

참가 물질

6

반응물 4

HCID 11430Potassium CarbonateHCID 25517Ammonium ChlorideHCID 709434,6-DichloropyrimidineHCID 66594500trans-2,6-dimethylhexahydro-1H-azepine hydrochloride

생성물 1

HCID 866074651-(6-chloropyrimidin-4-yl)-trans-2,6-dimethylhexahydro-1H-azepine수율 93.2%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
60 °C

실험 절차

Into 3 ml of acetonitrile were added 0.2 g of 4,6-dichloropyrimidine, 0.56 g of potassium carbonate and 0.31 g of trans-2,6-dimethylhexahydro-1H-azepine hydrochloride, and the mixture was stirred for 2 hours at 60° C. The reaction mixture was cooled to near room temperature, a saturated ammonium chloride aqueous solution was added therein, and the mixture was extracted with tert-butyl methyl ether three times. The organic layers were washed with a saturated sodium chloride aqueous solution, dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to silica gel column chromatography to obtain 0.30 g of 1-(6-chloropyrimidin-4-yl)-trans-2,6-dimethylhexahydro-1H-azepine.

후처리

  1. temperatureThe reaction mixture was cooled to near room temperature
  2. extractionthe mixture was extracted with tert-butyl methyl ether three times
  3. washThe organic layers were washed with a saturated sodium chloride aqueous solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-b9487ef63e354ac99b603e23139642a2
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07732448B2

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