Trifluoroacetic acid → HCID 68512974, 화합물

HRID 1716268노트

반응식

HRID 1716268 반응식
C(OC(=O)[NH:7][C@@H:8]1[CH2:14][CH:13]=[CH:12][CH2:11][N:10]([O:15][CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[C:9]1=[O:23])(C)(C)C.FC(F)(F)C(O)=O>ClCCl>[NH2:7][C@@H:8]1[CH2:14][CH:13]=[CH:12][CH2:11][N:10]([O:15][CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[C:9]1=[O:23]

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 68514761(1-benzyloxy-2-oxo-2,3,4,7-tetrahydro-1H-azepin-3-(R)-yl)-carbamic acid tert-butyl ester

생성물 1

HCID 68512974HCID 68512974, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 4.14 g (12.45 mmoles) of (1-benzyloxy-2-oxo-2,3,4,7-tetrahydro-1H-azepin-3-(R)-yl)-carbamic acid tert-butyl ester from Step C in 30 mL of dichloromethane was added 20 mL of trifluoroacetic acid. The reaction mixture was stirred for two hours at room temperature, and the solvent was removed under vacuum. Next, the reaction mixture was diluted in dichloromethane, and neutralized with NaHCO3(s). The reaction mixture was then extracted with NaHCO3(aq.) and NaCl (aq.) solutions. The aqueous layers were re-extracted with dichloromethane twice, and the organic layers combined and dried over Na2SO4(s). Filtration and solvent removal gave 3.685 g of a purple, viscous oil. MS: 465 (2M+H), 233 (M+H).

후처리

  1. customthe solvent was removed under vacuum
  2. additionNext, the reaction mixture was diluted in dichloromethane
  3. extractionThe reaction mixture was then extracted with NaHCO3(aq.) and NaCl (aq.) solutions
  4. extractionThe aqueous layers were re-extracted with dichloromethane twice
  5. dry with materialdried over Na2SO4(s)
  6. filtrationFiltration and solvent removal
  7. customgave 3.685 g of a purple, viscous oil

출처 및 근거

ORD 기록
ord-844f4b9d7272457f953544733d0bb126
출처 데이터셋
uspto-grants-2010_09
특허 번호
US07803793B2

반응 노트

불러오는 중…