HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylcarbamoyl Chloride → HCID 44200495, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylcarbamoyl Chloride | HCID 6598 | — |
| Reactant | HCID 59510479 | HCID 59510479 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 44200495 | HCID 44200495 | 93.3% |
Reaction Steps
To 4-amino-5-chloro-2-methoxy-N-[{4-(4-piperidinylmethyl)-2-morpholinyl}methyl]-benzamide (Example 23) (1.0 g) and a solution of TEA (0.53 ml) in methylene chloride (20 ml) was added dropwise dimethylcarbamoyl chloride (0.30 g) under ice-cooling. After completion of addition, the internal temperature of the reaction solution was warmed to room temperature, and the solution was stirred for 3 hours. The reaction solution was washed with water, then brine, and then dried over anhydrous magnesium sulfate. The solvent was removed in vacuo. The residue was purified by silica gel column chromatography (eluent: chloroform/methanol=30/1) to give the titled compound (1.1 g) as a white solid. Melting point 179-180° C. (recrystallized from EA)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07906510B2 |
| Source dataset | uspto-grants-2011_03 |
| ORD ID | ord-f96ddc64231d4468afb7e33893372087 |
| Source note | uspto-grants-2011_03 |