Pyridine → Trifluoromethanesulfonic acid 2-[4-((R)-3-dimethylaminopyrrolidin-1-yl)-3-fluorophenyl]-1-oxo-1,2,3,4-tetrahydroisoquinolin-6-yl ester

HRID 69414노트

반응식

HRID 69414 반응식
FC(F)(F)S([O:6][S:7]([C:10]([F:13])([F:12])[F:11])(=[O:9])=[O:8])(=O)=O.[CH3:16][N:17]([CH3:42])[C@@H:18]1[CH2:22][CH2:21][N:20]([C:23]2[CH:28]=[CH:27][C:26]([N:29]3[CH2:38][CH2:37][C:36]4[C:31](=[CH:32][CH:33]=[C:34](O)[CH:35]=4)[C:30]3=[O:40])=[CH:25][C:24]=2[F:41])[CH2:19]1.N1C=CC=CC=1>ClCCl>[CH3:16][N:17]([CH3:42])[C@@H:18]1[CH2:22][CH2:21][N:20]([C:23]2[CH:28]=[CH:27][C:26]([N:29]3[CH2:38][CH2:37][C:36]4[C:31](=[CH:32][CH:33]=[C:34]([O:6][S:7]([C:10]([F:11])([F:12])[F:13])(=[O:8])=[O:9])[CH:35]=4)[C:30]3=[O:40])=[CH:25][C:24]=2[F:41])[CH2:19]1

참가 물질

5

반응물 3

HCID 1049PyridineHCID 67749Trifluoromethanesulfonic anhydrideHCID 689879832-[4-((R)-3-Dimethylaminopyrrolidin-1-yl)-3-fluorophenyl]-6-hydroxy-3,4-dihydro-2H-isoquinolin-1-one

생성물 1

HCID 86635103Trifluoromethanesulfonic acid 2-[4-((R)-3-dimethylaminopyrrolidin-1-yl)-3-fluorophenyl]-1-oxo-1,2,3,4-tetrahydroisoquinolin-6-yl ester

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Trifluoromethanesulfonic anhydride (2.06 g) was added to a solution of 2-[4-((R)-3-dimethylaminopyrrolidin-1-yl)-3-fluorophenyl]-6-hydroxy-3,4-dihydro-2H-isoquinolin-1-one (1.5 g) and pyridine (0.64 g) in dichloromethane (40 mL) at 0° C. After 30 minutes, the mixture was partitioned between water and dichloromethane, and the organic phase was dried over magnesium sulfate and concentrated. The product with the molecular weight of 501.50 (C22H23F4N3O4S) was obtained in this way; MS (ESI): 502 (M+H+).

후처리

  1. customthe mixture was partitioned between water and dichloromethane
  2. dry with materialthe organic phase was dried over magnesium sulfate
  3. concentrationconcentrated
  4. customThe product with the molecular weight of 501.50 (C22H23F4N3O4S) was obtained in this way

출처 및 근거

ORD 기록
ord-8fd779e262d64cf6a87395e16586258a
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822495B2

반응 노트

불러오는 중…