Trifluoroacetic acid → HCID 53629854, 화합물
반응식
C(OC(=O)[NH:7][C@@H:8]1[CH2:12][CH2:11][N:10]([C:13]2[CH:18]=[CH:17][C:16]([Br:19])=[CH:15][N:14]=2)[CH2:9]1)(C)(C)C.C(O)(C(F)(F)F)=O>C(Cl)Cl>[Br:19][C:16]1[CH:17]=[CH:18][C:13]([N:10]2[CH2:11][CH2:12][C@@H:8]([NH2:7])[CH2:9]2)=[N:14][CH:15]=1참가 물질
4
실험 절차
Dissolve [(R)-1-(5-bromo-pyridin-2-yl)-pyrrolidin-3-yl]-carbamic acid tert-butyl ester (9.17 g, 26.9 mmol) in CH2Cl2 (45 mL), add TFA (10 mL) and stir at RT overnight. Remove the excess reagent in vacuo. Dilute the residue with CH2Cl2 (100 mL) and wash with 1.0 M NaOH (100 mL). Extract the aqueous layer with CH2Cl2 (3×100 mL). Combine the organic layers, dry with Na2SO4, filter and concentrate to give 6.03 g (93%) of the title compound. MS/ES m/z (79Br) 242 [M+H]+.
후처리
- customRemove the excess reagent in vacuo
- additionDilute the residue with CH2Cl2 (100 mL)
- washwash with 1.0 M NaOH (100 mL)
- extractionExtract the aqueous layer with CH2Cl2 (3×100 mL)
- dry with materialCombine the organic layers, dry with Na2SO4
- filtrationfilter
- concentrationconcentrate
출처 및 근거
- ORD 기록
- ord-98e6ab0732bd4e16bbd75fdceff59616
- 출처 데이터셋
- uspto-grants-2012_01
- 특허 번호
- US08101764B2
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