HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,2,2-Trichloroethyl chloroformate → HCID 15908473, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,2,2-Trichloroethyl chloroformate | HCID 87063 | — |
| Reactant | HCID 18768327 | HCID 18768327 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 15908473 | HCID 15908473 | 65.6% |
Reaction Steps
A solution of 11.5 g (33.29 mmol) of 1-{3-[benzyl(methyl)amino]propyl}-1,5,7,8-tetrahydro-2H-thiopyrano[4,3-d]pyrimidine-2,4-(3H)-dione in 200 ml of acetonitrile is treated with 7.92 g (36.63 mmol) of 2,2,2-trichloroethyl chloroformate, and the mixture is stirred at room temperature for 30 minutes. The solvent is then removed under reduced pressure and the residue is purified by column chromatography (silica gel, cyclohexane/ethyl acetate 1:1). This gives 9.4 g (63% yield) of a colourless solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06649618B2 |
| Source dataset | uspto-grants-2003_11 |
| ORD ID | ord-c27bd444482649f3a41478e10f58ed72 |
| Source note | uspto-grants-2003_11 |