HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 131723557, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 22036319 | HCID 22036319 | — |
| Product | HCID 131723557 | HCID 131723557 | 62% |
Reaction Steps
To a solution of the product obtained in Step 2 (0.43 g, 0.94 mmol) in CH2Cl2 (2 mL) was added CF3COOH (1.5 mL) at room temperature. The solution was stirred at room temperature for 5 h and evaporated to dryness. The residue was dissolved in EtOAc. The solution was washed with 25% aqueous NaOH and dried over K2CO3. A solution of HCl in Et2O was dropped into the solution until no more precipitate formed. The precipitate was collected, washed with ethyl ether, and dried in vacuum to give 251 mg (62%) of the title product: mp 158-160° C. MS m/z 358 (M)+. HRMS m/z calcd for C18H22N4O4 (M)+ 358.1641, found 358.1647.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07534794B2 |
| Source dataset | uspto-grants-2009_05 |
| ORD ID | ord-ab7ec4706b4f4cf9837eca0ad2d87b8c |
| Source note | uspto-grants-2009_05 |