Potassium Carbonate → 4-Acetamido-1-(6-methyl-2-pyridyl)piperidine

HRID 647512

반응식

HRID 647512 반응식
Cl[C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[N:3]=1.C(=O)([O-])[O-].[K+].[K+].[C:15]([NH:18][C:19]1[CH:24]=[CH:23][N:22]=[CH:21][CH:20]=1)(=[O:17])[CH3:16]>S1(CCCC1)(=O)=O>[C:15]([NH:18][CH:19]1[CH2:24][CH2:23][N:22]([C:2]2[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[N:3]=2)[CH2:21][CH2:20]1)(=[O:17])[CH3:16]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 21288N-Pyridin-4-ylacetamideHCID 876016-Chloro-2-picoline

생성물 1

HCID 129266184-Acetamido-1-(6-methyl-2-pyridyl)piperidine수율 28%

시약·촉매·용매 1

HCID 31347Sulfolane용매

실험 절차

0.042 mole of 2-chloro-6-methylpyridine, 0.056 mole of anhydrous potassium carbonate and 0.052 mole of 4-acetamidopyridine in 75 ml of sulfolane are heated to 150° C. with stirring for 24 hours, then the sulfolane is concentrated up to 1.5 of its volume, the mixture is poured into 100 ml of water and extraction is effected four times with 150 ml of diethyl ether. The organic phase is washed with water, it is dried over anhydrous sodium sulfate, concentrated to dryness and the residue is crystallised in 40 m of ethyl acetate. Thus, the 4-acetamido-1-(6-methyl-2-pyridyl)piperidine is obtained; m.p. 145° to 147° C.

후처리

  1. concentrationthe sulfolane is concentrated up to 1.5 of its volume
  2. additionthe mixture is poured into 100 ml of water and extraction
  3. washThe organic phase is washed with water, it
  4. dry with materialis dried over anhydrous sodium sulfate
  5. concentrationconcentrated to dryness
  6. customthe residue is crystallised in 40 m of ethyl acetate

출처 및 근거

ORD 기록
ord-a522ec499de54b678a31a66f02df464a
출처 데이터셋
uspto-grants-1983_10
특허 번호
US04409228

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