HuagongsheHuagongshe Chemistry Print Report · For research reference only
Disodium 2,3-dihydroxybutanedioate → HCID 86698315, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Disodium 2,3-dihydroxybutanedioate | HCID 13355 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | Diethylether water | HCID 21584184 | — |
| Reactant | HCID 86698314 | HCID 86698314 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86698315 | HCID 86698315 | — |
Reaction Steps
To a stirred solution of 1.28 g (4.1 mmol) 16β-azido-3-methoxy-estra-1,3,5(10)-triene in 30 ml abs. THF, 10 ml of a 1M lithium aluminum hydride solution in THF (Fluka) is added dropwise under cooling. The mixture is stirred for further 30 min at RT, followed by cautious addition of ether/water at 0° C. and subsequent addition of sodium tartrate solution. After three subsequent extractions of the aqueous phase with ether, the combined organic phases are washed twice with water, dried with sodium sulfate and concentrated. Yield after recrystallization from hexane: 1.05 g (89%), white solid matter with F=90-94° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09382288B2 |
| Source dataset | uspto-grants-2016_07 |
| ORD ID | ord-dba318140d62484a97d94b8b5b60f423 |
| Source note | uspto-grants-2016_07 |