Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Methanol | HCID 887 | — |
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | HCID 21201721 | HCID 21201721 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 21201864 | HCID 21201864 | 85.1% |
Reaction Steps
1-[1-(Pyrrolidin-1-ylcarbonylmethyl)-2-oxo-5-cyclohexyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepin-3-yl]-3-(4-ethoxycarbonylphenyl)urea was suspended in tetrahydrofuran (20 ml), aqueous lithium hydroxide (0.37 g) solution (10 ml) and methanol (20 ml) were added, the mixture was stirred at 40-50° C. for one hour. 1N hydrochloric acid and chloroform were added and extracted. The organic layer was washed with water and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, isopropyl ether was added to crystals so precipitated for trituration, collected by filtration, to thereby obtain 0.81 g of the title compound (Yield: 85.1%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06239131B1 |
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| Source dataset | uspto-grants-2001_05 |
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| ORD ID | ord-f917d4a95af8496198aefc1872a76005 |
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| Source note | uspto-grants-2001_05 |
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