HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 86698314, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Lithium azide | HCID 88163 | — |
| Reactant | HCID 67508166 | HCID 67508166 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 86698314 | HCID 86698314 | — |
Reaction Steps
A stirred solution of 1.56 g (4.5 mmol) 16α-bromo-3-methoxy-estra-1,3,5(10)-triene and 0.67 g (13.7 mmol) lithium azide in 30 ml of DMSO is heated for 1 h to 80° C. After cooling, water is added dropwise and the resulting precipitate is collected by filtration, washed with water and dried under vacuum. 1.33 g (96%). F=80-85° C., after recrystallization from ether/methanol: F=84-87° C. [α]D+60° (c=10.2).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09382288B2 |
| Source dataset | uspto-grants-2016_07 |
| ORD ID | ord-2a2a9d93fe004e60a2e0637b6a2778b5 |
| Source note | uspto-grants-2016_07 |