HCID 59457665, 화합물 → HCID 59457731, 화합물

HRID 1711096노트

반응식

HRID 1711096 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 101.9%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of the carboxylate 388 (1 g, 2.13 mmol) in DCM (4.3 mL) TFA (4.3 mL) was added and the reaction mixture was stirred 2 h at room temperature. The solvent was removed under reduced pressure, the residue was suspended in aqueous sodium bicarbonate, the mixture was extracted with DCM, EtOAc and DCM; the combined extracts were filtered and the recovered solids were collected and dried. The filtrate was dried over anhydrous Na2SO4, concentrated under reduced pressure and the residue was combined with the solid material obtained upon filtration, to afford 389 (806 mg, 100% yield) as a yellow solid. LCMS:(M+H) 372.1.

후처리

  1. customThe solvent was removed under reduced pressure
  2. extractionthe mixture was extracted with DCM, EtOAc and DCM
  3. filtrationthe combined extracts were filtered
  4. customthe recovered solids were collected
  5. customdried
  6. dry with materialThe filtrate was dried over anhydrous Na2SO4
  7. concentrationconcentrated under reduced pressure
  8. customobtained upon filtration

출처 및 근거

ORD 기록
ord-1db1c13ae1de406dbb8a411222b51d45
출처 데이터셋
uspto-grants-2010_09
특허 번호
US07790729B2

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