반응식
N#N.[Br:3][C:4]1[CH:5]=[C:6]([C:10](=[O:12])[CH3:11])[CH:7]=[CH:8][CH:9]=1.[CH2:13](O)[CH2:14][OH:15].COC(OC)OC.C([O-])([O-])=O.[Na+].[Na+]>>[Br:3][C:4]1[CH:5]=[C:6]([C:10]2([CH3:11])[O:15][CH2:14][CH2:13][O:12]2)[CH:7]=[CH:8][CH:9]=1참가 물질
6
반응 조건
- 온도
- 95 °C
실험 절차
In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a solution of 1-(3-bromo-phenyl)-ethanone (1360 mg, 6.83 mmol) in ethylene glycol (8.00 mL, 143.46 mmol) was treated with trimethylorthoformate (1.50 mL, 13.68 mmol) followed by LiBF4 (131 mg, 1.37 mmol). The reaction mixture was heated at 95° C. for 15 h. Sat. aq. Na2CO3 was added and the mixture was extracted twice with ether and the combined organic extracts were dried over Na2SO4, filtered, and the solvent was removed under reduced pressure. Purification of the residue by FC (20:1 hept-EA) gave the title compound as a pale yellow oil: TLC:rf (10:1 hept-EA)=0.34. LC-MS-conditions 02: tR=1.01 min.
후처리
- extractionthe mixture was extracted twice with ether
- dry with materialthe combined organic extracts were dried over Na2SO4
- filtrationfiltered
- customthe solvent was removed under reduced pressure
- customPurification of the residue by FC (20:1 hept-EA)
출처 및 근거
- ORD 기록
- ord-2395729cc9094f8db19164bab0b1ef65
- 출처 데이터셋
- uspto-grants-2013_09
- 특허 번호
- US08536209B2
연결된 노트
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