HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 1,2,3,10,11,11a-Hexahydro-9,11-dihydroxy-8-methyl-5H-pyrrolo(2,1-c)(1,4)benzodiazepin-5-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | HCID 13567463 | HCID 13567463 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 1,2,3,10,11,11a-Hexahydro-9,11-dihydroxy-8-methyl-5H-pyrrolo(2,1-c)(1,4)benzodiazepin-5-one | HCID 153354 | — |
Reaction Steps
64.4 mg of 2,3,5,11a-tetrahydro-9-hydroxy-8-methyl-1H-pyrrolo(2,1-C)(1,4)benzodiazepin-5-one was dissolved in 2.5 ml of hot acetonitrile, 0.5 ml of water was added thereto, and the mixture was allowed to stand first at room temperature for 2 hours and then at -20° C. for 1 day. Thus, 51.1 mg of 2,3,5,10,11,11a-hexahydro-9,11-dihydroxy-8-methyl-1H-pyrrolo(2,1-C)(1,4)benzodiazepin-5-one was obtained as a yellow-colored crystal. Recrystallization of the resulting product from aqueous acetonitrile gave a yellow-colored prismatic crystal having a melting point of 154° to 156° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04239683 |
| Source dataset | uspto-grants-1980_12 |
| ORD ID | ord-346a23a1ef59439c93eb4108e4dda5dc |
| Source note | uspto-grants-1980_12 |