3,4-diMethylbenzo[d]oxazol-2(3H)-one synthesis
- Product Name:3,4-diMethylbenzo[d]oxazol-2(3H)-one
- CAS Number:67932-16-5
- Molecular formula:C9H9NO2
- Molecular Weight:163.17
74-88-4
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Yield:67932-16-5 82%
Reaction Conditions:
Stage #1: 4-methyl-3H-benzooxazol-2-onewith potassium tert-butylate in tetrahydrofuran at 20; for 0.5 h;
Stage #2: methyl iodide in tetrahydrofuran at 20;
Steps:
4.4a
4a) 3,4-dimethyl-3H-benzoxazol-2-one A solution of 10.0 g (67.0 mmol) 4-methyl-3H-benzoxazol-2-one in 200 mL THF was combined with 8.0 g (70.6 mmol) potassium-tert.-butoxide, stirred for 30 min at RT, then combined with 7.0 mL (110.3 mmol) iodomethane and stirred overnight at RT. The reaction mixture was combined with 100 mL EtOAc, washed twice with 50 mL saturated NaCl solution, the organic phase was dried over MgSO4, filtered and evaporated to dryness i.vac. The residue was combined with PE/EtOAc 2:1, the precipitate was suction filtered and dried at 60° C. in the vacuum drying cupboard. Yield: 9.0 g (82% of theory) ESI-MS: (M+H)+=164 Rf=0.56 (silica gel, PE/EtOAc 2:1)
References:
US2005/256099,2005,A1 Location in patent:Page/Page column 175
![4-methylbenzo[d]oxazol-2(3H)-one](/CAS/GIF/78258-80-7.gif)
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