HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → 4,5-Pyrimidinediamine, 6-chloro-
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | 5-Amino-4,6-dichloropyrimidine | HCID 79434 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 4,5-Pyrimidinediamine, 6-chloro- | HCID 78010 | 71% |
Reaction Conditions
| Temperature | 100 °C |
|---|
Reaction Steps
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).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09440978B2 |
| Source dataset | uspto-grants-2016_09 |
| ORD ID | ord-6fbcc52a42154b628a7afb18ebbb138a |
| Source note | uspto-grants-2016_09 |