HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl chloroformate → HCID 13450726, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl chloroformate | HCID 10928 | — |
| Reactant | 2H-1,4-Benzodiazepin-2-one, 1,3-dihydro-1-(1-methyl-4-piperidinyl)-5-phenyl- | HCID 56658 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Solvent | Benzene | HCID 241 | — |
| Product | HCID 13450726 | HCID 13450726 | 100.4% |
Reaction Steps
A solution of 98 mg (0.29 mmol) of 1,3-dihydro-1-(1-methyl-4-piperidinyl)-5-phenylbenzodiazepin-2-one 3, 0.084 ml (0.29×3 mmol) of ethyl chloroformate and 54.3 mg (0.29×2.2 mmol) of sodium hydrogencarbonate in 5 ml of benzene is refluxed under heating for 7 hours. The reaction mixture is poured into ice water and extracted with methylene chloride. The organic layer is washed with water dried over anhydrous magnesium sulfate and concentrated to give 114 mg of 1-(1-ethoxycarbonyl-4-piperidinyl)-1,3-dihydro-5-phenyl-2H-1,4-benzodiazepin-2-one 12 as powders. The yield is 100%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04579685 |
| Source dataset | uspto-grants-1986_04 |
| ORD ID | ord-658a4ded9abb4cba9f373e94aa2792b3 |
| Source note | uspto-grants-1986_04 |