HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Chloroethyl chloroformate → HCID 118023935, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Chloroethyl chloroformate | HCID 521305 | — |
| Reactant | HCID 118024028 | HCID 118024028 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Product | HCID 118023935 | HCID 118023935 | 77.3% |
Reaction Steps
To a mixture of 5-benzyl-2-[(6-cyclohexyl-2-methylthieno[2,3-d]pyrimidin-4-yl)methyl]-2,5-diazabicyclo[2.2.2]octan-3-one (140 mg) and DCE (5 mL) was added 1-chloroethyl chloroformate (50 μL), followed by stirring at room temperature overnight. The reaction solution was purified by silica gel column (chloroform/MeOH/saturated aqueous NH3) without concentration. The residue was dissolved in MeOH, and heated to reflux for 30 minutes. The reaction mixture was concentrated under reduced pressure and the residue was purified by silica gel column (chloroform/MeOH/saturated aqueous NH3) to obtain 2-[(6-cyclohexyl-2-methylthieno[2,3-d]pyrimidin-4-yl)methyl]-2,5-diazabicyclo[2.2.2]octan-3-one (87 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09051339B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-23df4249bd4d4e7195ad4fb50769ee47 |
| Source note | uspto-grants-2015_06 |