反应 #3266

反应方程式

4-Methylamino-2-methylsulfanyl-5-pyrimidine-methanol

sodium dichromate-dihydrate

sodium dichromate-dihydrate

→

4-methylamino-2-methylsulfanyl-5-pyrimidinecarboxaldehyde

收率 30.2%

溶剂

acetic acid

acetic acid

acetic acid

反应条件

后处理

1. 1
   其他After a total reaction time of 3.5 hours, the bright yellow solid was removed by filtration
2. 2
   workup.ADDITIONWater (30 mL) was added to the filtrate
3. 3
   温度The mixture was cooled in the refrigerator for 30 minutes
4. 4
   其他The precipitate was collected
5. 5
   workup.DISSOLUTIONdissolved in ethyl acetate
6. 6
   干燥the solution was dried over MgSO4
7. 7
   过滤Filtration and concentration in vacuo

实验过程

4-Methylamino-2-methylsulfanyl-5-pyrimidine-methanol (2.40 g, 13.0 mmol) in 7 mL of acetic acid was added to a solution of sodium dichromate-dihydrate (1.30 g, 4.4 mmol) in 6 mL of acetic acid. After 2 hours at room temperature, additional sodium dichromate-dihydrate (0.3 g, 1.0 mmol) in 1 mL of acetic acid was added. After a total reaction time of 3.5 hours, the bright yellow solid was removed by filtration. Water (30 mL) was added to the filtrate, followed by aqueous ammonium hydroxide until basic (pH 9.0). The mixture was cooled in the refrigerator for 30 minutes. The precipitate was collected and dissolved in ethyl acetate, and the solution was dried over MgSO4. Filtration and concentration in vacuo gave 0.72 g (30%) of 4-methylamino-2-methylsulfanyl-5-pyrimidinecarboxaldehyde; mp 99°-101° C.

来源