反应详情

温度

0 °C

A suspension of 6-cyclopropyl-2-(methylsulfonyl)pyrimidine-4-carboxylic acid (200 mg, 0.82 mmol) in dichloromethane (2 mL) and methanol (0.5 mL) was cooled to 0° C. Trimethylsilyl diazomethane (2.0 M in diethyl ether, 1.0 mL, 2.0 mmol) was added dropwise as not to increase the internal temperature of the reaction. Upon complete addition the suspension became a yellow colored solution that was allowed to warm to RT and maintained for 1 h at that temperature. At this time, acetic acid was added dropwise until the mixture was colorless (c.a. 2 drops, 12 M) and the resulting solution was concentrated under vacuum to a residue. The resulting oily yellow solid was dissolved in sparing ice cold acetonitrile (0.5 mL) and allowed to precipitate to furnish an off white waxy solid. MS m/z 257.1 (M+1). 1H NMR (400 MHz, DMSO-d6): δ 8.22 (s, 1H), 3.81 (s, 3H), 3.28 (s, 3H), 2.40-2.36 (m, 1H), 1.20-1.15 (m, 2H), 1.12-1.06 (m, 2H).

1. temperatureto increase
2. customthe internal temperature of the reaction
3. additionUpon complete addition the suspension
4. temperatureto warm to RT
5. temperaturemaintained for 1 h at that temperature
6. concentrationthe resulting solution was concentrated under vacuum to a residue
7. dissolutionThe resulting oily yellow solid was dissolved in sparing ice cold acetonitrile (0.5 mL)
8. customto precipitate
9. customto furnish an off white waxy solid