HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl chloroformate → HCID 69288561, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl chloroformate | HCID 6586 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 11531195 | HCID 11531195 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 69288561 | HCID 69288561 | — |
Reaction Steps
tert-Butyl 5-amino-2-methylthio-4-(3-hydroxyphenyl)-thieno[2,3-d]pyrimidine-6-carboxamide (example 1f, 100 mg) was dissolved in dry CH2Cl2 (5 ml). DIPEA (500 μl ) and methyl chloroformate (199 μl ) were added and the reaction mixture was stirred at room temperature overnight. The reaction mixture was washed with H2O. The organic layer was dried (MgSO4) and concentrated under reduced pressure. The title compound was purified by HPLC using a Luna C-18 column with the following gradient: CH3CN/H2O=10/90 to 90/10 (v/v) in 30 min. The title compound was then lyophilized from a mixture of 1,4-dioxane and H2O.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07229990B2 |
| Source dataset | uspto-grants-2007_06 |
| ORD ID | ord-0b17191c13f04d329ba3cdcc398a91d4 |
| Source note | uspto-grants-2007_06 |