HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 54232406, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | Methyl 7-carboxy-2,3,4,5-tetrahydro-4-methyl-3-oxo-1h-1,4-benzodiazepine-2-acetate | HCID 23505570 | — |
| Product | HCID 54232406 | HCID 54232406 | 63% |
Reaction Steps
EDC (759 mg, 3.96 mmol) was added to a solution of the compound of Preparation BB(b) (3.6 mmol), methyl (±)-7-carboxy-2,3,4,5-tetrahydro-4-methyl-3-oxo-1H-1,4-benzodiazepine-2-acetate (1.05 g, 3.6 mmol), HOBT.H2O (535 mg, 3.96 mmol), and DIEA (2.07 mL, 11.88 mmol) ion anhydrous DMF at RT. After 20 h, the reaction was concentrated, and the residue was dissolved in CH2Cl2 and chromatographed (silica gel, step gradient 0-10%, CH3OH/CH2Cl2) to give the title compound as a pale yellow solid (960 mg, 63%): MS(ES) m/e 427 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06159964 |
| Source dataset | uspto-grants-2000_12 |
| ORD ID | ord-5f07beb4ba5f403682699c36f81e6fb2 |
| Source note | uspto-grants-2000_12 |