Ammonia → 4,5-Pyrimidinediamine, 6-chloro-

Temperatur

100 °C

To a 7 N solution of ammonia in MeOH (40 mL) was added 4,6-dichloropyrimidin-5-ylamine (8.7 g, 53 mmol) and the solution was heated to 100° C. in a sealed tube. After 12 h, the resulting solution was cooled to rt and allowed to stand for 2 h. The colorless crystalline material that resulted was collected by filtration and washed with ice cold MeOH (10 mL) to give the title compound (5.4 g, 71%). MS (ESI): mass calcd. for C4H5ClN4, 144.0; m/z found, 145.0 [M+H]+. 1H NMR ((CD3)250): 7.64 (s, 1H), 6.70 (s, 2H), 4.93 (s, 2H).

1. temperaturethe resulting solution was cooled to rt
2. waitto stand for 2 h
3. customThe colorless crystalline material that resulted
4. filtrationwas collected by filtration
5. washwashed with ice cold MeOH (10 mL)

ORD-Eintrag

ord-6fbcc52a42154b628a7afb18ebbb138a

Quelldatensatz

uspto-grants-2016_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09440978B2