HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → HCID 20359983, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Bromine | HCID 24408 | — |
| Reactant | HCID 20359979 | HCID 20359979 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 20359983 | HCID 20359983 | 89.2% |
Reaction Steps
A solution of 6.4 g of bromine (0.04 mol) in 30 ml of methylene chloride is added dropwise over the course of one hour to a solution of 8.5 g (0.04 mol) of 2-ethylamino-4-cyclopropylamino-6-chloropyrimidine in 300 ml of methylene chloride, whilst cooling with ice. The solution is left to stand overnight at room temperature, 150 ml of water are then added and the mixture is brought to pH 9-10 with dilute ammonia solution. The organic phase is separated off, rinsed with water, dried over magnesium sulphate, filtered and evaporated. The evaporation residue (12 g), when recrystallised from methanol-water (1:1), gives 10.4 g of colourless crystals of melting point 100°-101°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04082535 |
| Source dataset | uspto-grants-1978_04 |
| ORD ID | ord-4957b545e1784b40b7213ce57b1de86d |
| Source note | uspto-grants-1978_04 |