反应详情

To 10 ml of a 1 N methanolic sodium methoxide solution are added dropwise 3 ml of a 3.5 N methanolic methylmercaptan solution. To the resultant methylmercaptide solution is added a solution of 2.01 g (0.01 mole) of methyl 2-methoxy-6-chloronicotinate (cf. Example 6 a)) in 30 ml of methanol. The reaction mixture is refluxed for 5 hours and the solvent is thereafter evaporated in vacuo. The residue is treated with 30 ml of saturated potassium carbonate solution and 150 ml of methylene chloride and separated in a separating funnel. The methylene chloride solution is dried over sodium sulphate and subsequently evaporated to dryness in vacuo. The crystallised residue is recrystallised from pentane and yields the methyl 2-methoxy-6-(methylthio)-nicotinate with a melting point of 71°-75° C.

1. temperatureThe reaction mixture is refluxed for 5 hours
2. customthe solvent is thereafter evaporated in vacuo
3. additionThe residue is treated with 30 ml of saturated potassium carbonate solution and 150 ml of methylene chloride
4. customseparated in a separating funnel
5. dry with materialThe methylene chloride solution is dried over sodium sulphate
6. customsubsequently evaporated to dryness in vacuo
7. customThe crystallised residue is recrystallised from pentane