Dimethylformamide → BOC-aminoether
반응식
[C:1](OC(N1CCC(O)CC1)=O)([CH3:4])([CH3:3])[CH3:2].[C:15](=[O:18])([O-:17])[O-:16].[Cs+].[Cs+].C[N:22](C=O)C>FC1C=CC(C(F)(F)F)=CC=1>[C:15]([O:17][NH2:22])([O:16][C:1]([CH3:4])([CH3:3])[CH3:2])=[O:18]참가 물질
5
실험 절차
Part A: A solution of N-(tert-butyloxycarbonyl)-4-piperidinol (5.00 g, 2.48 mmol), 4-fluorobenzo-trifluoride (3.46 mL, 2.73 mmol), and cesium carbonate (12.1 g, 3.72 mmol) in DMF (60 mL) was heated at 120° C. under N2 for 2 days. The mixture was concentrated, diluted with H2O, and extracted with ethyl acetate. The organic layer was washed with H2O and brine, dried with MgSO4, and concentrated in vacuo. Chromatography (on silica, ethyl acetate/hexane) provided the BOC-aminoether as a white solid (6.97 g, 81%); Anal. calculated. for C17H22NO3F3: C, 59.12; H, 6.42; N, 4.06. Found: C, 59.29; H, 6.47; N, 3.99.
후처리
- concentrationThe mixture was concentrated
- additiondiluted with H2O
- extractionextracted with ethyl acetate
- washThe organic layer was washed with H2O and brine
- dry with materialdried with MgSO4
- concentrationconcentrated in vacuo
출처 및 근거
- ORD 기록
- ord-3a987048a39445208ab700af7944adbf
- 출처 데이터셋
- uspto-grants-2004_02
- 특허 번호
- US06696449B2
반응 노트
불러오는 중…