HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → HCID 44409937, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Sodium Dithionite | HCID 24489 | — |
| Reactant | HCID 44409787 | HCID 44409787 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 44409937 | HCID 44409937 | 30% |
Reaction Steps
To a suspension of 6-(1-azepanyl)-N,2-dicyclopropyl-5-nitro-4-pyrimidinamine 197 (0.5 g, 16 mmol) in 1,4-dioxane (35 ml) and water (35 ml) is added sodium hydrosulfite (2.19 g, 13 mmol) and ammonia (25% solution, 1.2 ml). The mixture is stirred at room temperature for 10 h then diluted with ethyl acetate and washed three times with water. The combined organic layers are dried over magnesium sulfate and concentrated in vacuo to afford a yellow oil. The crude oil is purified by column chromatography (dichloromethane/ethanol/ammonia: 95/5/0.5) to give pure 6-(1-azepanyl)-N4,2-dicyclopropyl-4,5-pyrimidinediamine 63 (137 mg, 30%) as a reddish solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07544675B2 |
| Source dataset | uspto-grants-2009_06 |
| ORD ID | ord-3c456d309596444ebd0d37ae13530fb9 |
| Source note | uspto-grants-2009_06 |