Trimethylsilyldiazomethane → Methyl 2-amino-4-bromo-3-methylbenzoate
반응식
[CH3:1][Si](C=[N+]=[N-])(C)C.[NH2:8][C:9]1[C:17]([CH3:18])=[C:16]([Br:19])[CH:15]=[CH:14][C:10]=1[C:11]([OH:13])=[O:12]>C(OCC)(=O)C.C(O)C>[NH2:8][C:9]1[C:17]([CH3:18])=[C:16]([Br:19])[CH:15]=[CH:14][C:10]=1[C:11]([O:13][CH3:1])=[O:12]참가 물질
5
실험 절차
Add (trimethylsilyl)diazomethane (16.5 mL, 33 mmol, 2 M in hexane) to a solution of 2-amino-4-bromo-3-methyl-benzoic acid (3.8 g, 16.5 mmol) in ethyl acetate (50 mL) and ethanol (50 mL) at room temperature and stir the solution for 16 h. Remove the solvent under reduced pressure. Chromatograph the residue over silica gel, eluting with hexanes/ethyl acetate, to afford the title compound (3.54 g, 88%). MS (ES+): 245 (M+H).
후처리
- customRemove the solvent under reduced pressure
- washChromatograph the residue over silica gel, eluting with hexanes/ethyl acetate
출처 및 근거
- ORD 기록
- ord-6ab3e58b2d5844cf904791881b1e8bb0
- 출처 데이터셋
- uspto-grants-2010_08
- 특허 번호
- US07786108B2
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