HCID 59605970, 화합물 → (4-Methylpiperidin-4-yl)(pyrrolidin-1-yl)methanone

HRID 1922643노트

반응식

HRID 1922643 반응식
C(OC([N:8]1[CH2:13][CH2:12][C:11]([CH3:21])([C:14]([N:16]2[CH2:20][CH2:19][CH2:18][CH2:17]2)=[O:15])[CH2:10][CH2:9]1)=O)(C)(C)C>C(O)(C(F)(F)F)=O.C(Cl)Cl.O>[CH3:21][C:11]1([C:14]([N:16]2[CH2:20][CH2:19][CH2:18][CH2:17]2)=[O:15])[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]1

참가 물질

5

반응물 1

HCID 59605970HCID 59605970, 화합물

생성물 1

HCID 24728852(4-Methylpiperidin-4-yl)(pyrrolidin-1-yl)methanone수율 99.9%

시약·촉매·용매 3

HCID 962Water용매HCID 6344Dichloromethane용매HCID 6422Trifluoroacetic acid용매

실험 절차

A solution of 4-methyl-4-(pyrrolidine-1-carbonyl)piperidine-1-carboxylic acid tert-butyl ester (296 mg, 1.0 mmol) in TFA (5 mL), DCM (5 mL) and water (0.1 mL) was stirred at room temperature for 2 hours and then concentrated under reduced pressure. The residue was taken up in MeOH and and loaded onto an Isolute® SCX-2 cartridge (10 g). The cartridge was washed with MeOH and the desired product was eluted with 2M NH3 in MeOH. The solvents were removed to give the desired product as a white solid (196 mg, 66%). LCMS (Method A): RT 0.31 min; [M+H]+ 197

후처리

  1. concentrationconcentrated under reduced pressure
  2. washThe cartridge was washed with MeOH
  3. washthe desired product was eluted with 2M NH3 in MeOH
  4. customThe solvents were removed

출처 및 근거

ORD 기록
ord-4758a1b8804a4bda82877480d23aabd0
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08173650B2

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