反应详情

N-Nitroso-N-benzyl-p-toluene sulphonamide (966 mg, 3.33 mmol) was added in small portions to a solution of sodium methoxide (2.0 ml of 2M solution in methanol) in t-butyl methyl ether (12 ml) and methanol (2 ml) at room temperature. After the addition was finished the reaction mixture was refluxed for 15-30 min. The reaction mixture was cooled and washed with water (3×6 ml). The ethereal solution of phenyl diazomethane was dried over sodium sulphate for 30 minutes. The solvent was removed in vacuo and the residue distilled under reduce pressure to give phenyl diazomethane as a dark red oil (30% yield, b.p. 20° C. at 1 mmHg) which was immediately dissolved in t-butyl methyl ether (6 ml).

1. additionAfter the addition
2. temperaturewas refluxed for 15-30 min
3. temperatureThe reaction mixture was cooled
4. washwashed with water (3×6 ml)
5. dry with materialThe ethereal solution of phenyl diazomethane was dried over sodium sulphate for 30 minutes
6. customThe solvent was removed in vacuo
7. distillationthe residue distilled