Potassium Carbonate → N-(5-bromo-3-methyl-pyridin-2-yl)-2-pyrrolidin-1-yl-acetamide

HRID 1916741

반응식

HRID 1916741 반응식
[NH:1]1[CH2:5][CH2:4][CH2:3][CH2:2]1.[Br:6][C:7]1[CH:8]=[C:9]([CH3:18])[C:10]([NH:13][C:14](=[O:17])[CH2:15]Cl)=[N:11][CH:12]=1.C([O-])([O-])=O.[K+].[K+]>CN(C=O)C.O>[Br:6][C:7]1[CH:8]=[C:9]([CH3:18])[C:10]([NH:13][C:14](=[O:17])[CH2:15][N:1]2[CH2:5][CH2:4][CH2:3][CH2:2]2)=[N:11][CH:12]=1

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 31268PyrrolidineHCID 52228026n-(5-Bromo-3-methyl-pyridin-2-yl)-2-chloro-acetamide

생성물 1

HCID 67362705N-(5-bromo-3-methyl-pyridin-2-yl)-2-pyrrolidin-1-yl-acetamide

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

0.81 mL (9.9 mmol) pyrrolidine are added to a suspension of 2.37 g (9.0 mmol) N-(5-bromo-3-methyl-pyridin-2-yl)-2-chloro-acetamide and 2.49 g (18 mmol) K2CO3 in 22.5 mL DMF and the reaction mixture is stirred for 20 h at RT. It is diluted with water, extracted exhaustively with EtOAc, the combined organic phases are washed with water and dried over Na2SO4. After the desiccant and solvent have been eliminated the residue is taken up in a little diisopropylether, cooled to 0° C., the crystals precipitated are suction filtered and dried in the air.

후처리

  1. extractionextracted exhaustively with EtOAc
  2. washthe combined organic phases are washed with water
  3. dry with materialdried over Na2SO4
  4. temperaturecooled to 0° C.
  5. customthe crystals precipitated
  6. filtrationare suction filtered
  7. customdried in the air

출처 및 근거

ORD 기록
ord-c0b803486c1f41659abfeb3b7564a30c
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08618132B2

연결된 노트

불러오는 중…