HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 178452973, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | 2-Bromo-2'-nitroacetophenone | HCID 244025 | — |
| Reactant | Tert-butyl amino(imino)methylcarbamate | HCID 86691067 | — |
| Product | HCID 178452973 | HCID 178452973 | 36% |
Reaction Steps
tert-Butyl amino(imino)methylcarbamate (4.78 g; 30 mmol) was dissolved in N,N-dimethylformamide (30 mL), 2-bromo-2′-nitroacetophenone (2.44 g; 10 mmol) was added thereto, and the mixture was stirred for 144 hours at room temperature. To the reaction solution, water (100 mL) was added, and the precipitated powder was collected by filtration. The resulting powder was dissolved in ethyl acetate (200 mL), and the mixture was washed with saturated aqueous sodium bicarbonate solution (two times). The organic layer was dried over anhydrous magnesium sulfate and then distilled under reduced pressure. The resulting residue was dispersed in acetone/diethyl ether, collected by filtration and dried to give 1.09 g of the title compound (yield 36%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08975411B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-c3eebfe086a849e58b6c7c1c0b55b0db |
| Source note | uspto-grants-2015_03 |