HCID 59457665, 화합물 → HCID 59457731, 화합물

HRID 418684노트

반응식

HRID 418684 반응식
[F:1][C:2]1[CH:30]=[C:29]([N+:31]([O-:33])=[O:32])[CH:28]=[CH:27][C:3]=1[O:4][C:5]1[CH:10]=[CH:9][N:8]=[C:7]2[CH:11]=[C:12]([C:14]3[CH2:19][CH2:18][N:17](C(OC(C)(C)C)=O)[CH2:16][CH:15]=3)[S:13][C:6]=12>C(Cl)Cl>[F:1][C:2]1[CH:30]=[C:29]([N+:31]([O-:33])=[O:32])[CH:28]=[CH:27][C:3]=1[O:4][C:5]1[CH:10]=[CH:9][N:8]=[C:7]2[CH:11]=[C:12]([C:14]3[CH2:19][CH2:18][NH:17][CH2:16][CH:15]=3)[S:13][C:6]=12

참가 물질

3

반응물 1

HCID 59457665HCID 59457665, 화합물

생성물 1

HCID 59457731HCID 59457731, 화합물수율 100%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of tert-butyl 4-(7-(2-fluoro-4-nitrophenoxy)thieno[3,2-b]pyridin-2-yl)-5,6-dihydropyridine-1(2H)-carboxylate 267 (1 g, 2.13 mmol) in DCM (4.3 mL) TFA (4.3 mL) was added and the reaction mixture was stirred for 2 h at room temperature. The solvent was removed under reduced pressure, the residue was suspended in aqueous sodium bicarbonate, the mixture extracted with DCM, EtOAc and DCM; the combined organic phases were filtered and the recovered solids dried. The organic phase was dried over anhydrous Na2SO4, concentrated under reduced pressure and the residue was combined with the solid material obtained earlier to provide 268 (806 mg, 2.12 mmol, 100% yield) as a yellow solid. MS (m/z): (M+1) 372.1 (100%).

후처리

  1. customThe solvent was removed under reduced pressure
  2. extractionthe mixture extracted with DCM, EtOAc and DCM
  3. filtrationthe combined organic phases were filtered
  4. customthe recovered solids dried
  5. dry with materialThe organic phase was dried over anhydrous Na2SO4
  6. concentrationconcentrated under reduced pressure
  7. customobtained earlier

출처 및 근거

ORD 기록
ord-97658b1d5ebf47a2a3d51808a9088cd9
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08093264B2

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