HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 67155029, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | tert-Butyldiphenylchlorosilane | HCID 94078 | — |
| Reactant | HCID 67155001 | HCID 67155001 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 67155029 | HCID 67155029 | — |
Reaction Steps
17-(cyclopropylmethyl)-4,5a-epoxy-3,14-dihydroxy-6-(1,3-dioxolan-2-yl)morphinan (3.85 g, 10 mmol) was dissolved in 10 ml of THF, then triethylamine (1.01 g, 10 mmol) and tert-butyldiphenyl chlorosilane (2.75 g, 10 mmol) were added with stirring. The whole system was reacted at a temperature ranging from 45° C. to 50° C. for 2 hours. After the reaction was complete, water was added to the system and the resultant mixture was extracted with diethyl ether for 3 times. The organic layer was washed with water, dried over anhydrous magnesium sulfate, and concentrated for crystallization to afford a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08563721B2 |
| Source dataset | uspto-grants-2013_10 |
| ORD ID | ord-bfac5af1e6f3487d83fe3bfd73484f19 |
| Source note | uspto-grants-2013_10 |