Potassium Carbonate → tert-butyl 2-(5'-bromo-3,4,5,6-tetrahydro-2H-[1,2]bipyridinyl-4-yl)ethylcarbamate

HRID 1019694

반응식

HRID 1019694 반응식
Br[C:2]1[CH:7]=[CH:6][C:5]([Br:8])=[CH:4][N:3]=1.[NH:9]1[CH2:14][CH2:13][CH:12]([CH2:15][CH2:16][NH:17][C:18](=[O:24])[O:19][C:20]([CH3:23])([CH3:22])[CH3:21])[CH2:11][CH2:10]1.C(=O)([O-])[O-].[K+].[K+].C(=O)([O-])O.[Na+]>C(Cl)(Cl)Cl>[Br:8][C:5]1[CH:6]=[CH:7][C:2]([N:9]2[CH2:14][CH2:13][CH:12]([CH2:15][CH2:16][NH:17][C:18](=[O:24])[O:19][C:20]([CH3:22])([CH3:21])[CH3:23])[CH2:11][CH2:10]2)=[N:3][CH:4]=1

참가 물질

6

반응물 4

HCID 11430Potassium CarbonateHCID 693532,5-DibromopyridineHCID 516892Sodium BicarbonateHCID 15018494-(2-Aminoethyl)piperidine, 4-BOC protected

생성물 1

HCID 66661183tert-butyl 2-(5'-bromo-3,4,5,6-tetrahydro-2H-[1,2]bipyridinyl-4-yl)ethylcarbamate

시약·촉매·용매 1

HCID 6212Chloroform용매

반응 조건

온도
130 °C

실험 절차

10.37 g (43.80 mmol) of 2,5-dibromopyridine, 10.00 g (43.80 mmol) of tert-butyl 2-piperidin-4-ylethylcarbamate and 6.05 g (43.80 mmol) of potassium carbonate are placed in an autoclave. The mixture is then heated at 130° C. for 12 hours. The reaction mixture is allowed to cool to room temperature and then taken up in chloroform and saturated aqueous sodium hydrogen carbonate solution. The aqueous phase is separated out and extracted twice with chloroform, and the combined organic phases are washed with saturated aqueous sodium chloride solution and dried over sodium sulfate, and the filtrate is concentrated under reduced pressure.

후처리

  1. temperatureto cool to room temperature
  2. customThe aqueous phase is separated out
  3. extractionextracted twice with chloroform
  4. washthe combined organic phases are washed with saturated aqueous sodium chloride solution
  5. dry with materialdried over sodium sulfate
  6. concentrationthe filtrate is concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-dab2bd828e60411a9ec5e24385c50ac9
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08716289B2

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