Trifluoroacetic acid → HCID 53629854、化合物
反応式
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]=1参加物
4
実験手順
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]+.
後処理
- 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
出典と根拠
- ORDレコード
- ord-98e6ab0732bd4e16bbd75fdceff59616
- 出典データセット
- uspto-grants-2012_01
- 特許番号
- US08101764B2
反応ノート
読み込み中…