Ammonia → 6-Chloro-2-methylpyrimidine-4,5-diamine

Temperature

150 °C

A 200 mL stainless steel Parr vessel was loaded with 5-amino-4,6-dichloro-2-methylpyrimidine (7.2 g, 40 mmol) and 2 M ammonia in isopropanol (100 mL), and then was sealed and heated at 150° C. for 16 h. HPLC analysis indicated complete conversion. The mixture was concentrated in vacuo, and the residue was suspended in a mixture of H2O (10 mL) and isopropanol (35 mL). This was stirred at 50° C. for 1 h and then was cooled to room temperature. The precipitate was collected by suction filtration, washed sparingly with isopropanol, then air dried on the filter to afford 6-chloro-4,5-diamino-2-methylpyrimidine (5.8 g, 91%) as a brown powder, which was used without further purification in the next step.

1. customwas sealed
2. concentrationThe mixture was concentrated in vacuo
3. additionthe residue was suspended in a mixture of H2O (10 mL) and isopropanol (35 mL)
4. temperaturewas cooled to room temperature
5. filtrationThe precipitate was collected by suction filtration
6. washwashed sparingly with isopropanol
7. customair dried on the
8. filtrationfilter

ORD record

ord-e243258ad81a4b0185dda7b3f4dc6261

Source dataset

uspto-grants-2014_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08895568B2