HuagongsheHuagongshe Chemistry Print Report · For research reference only
Bromine → HCID 131710459, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Bromine | HCID 24408 | — |
| Reactant | HCID 86733283 | HCID 86733283 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 131710459 | HCID 131710459 | — |
Reaction Steps
A solution of 3α-hydroxy-2β-methyl-5α-pregnane-11,20-dione (1.04g.) in dry methanol (150ml) was stirred at 0°-5° during the dropwise addition of a solution of bromine (0.16ml) in dry methanol (20ml) over a period of 2.5 hours. The reaction mixture was partitioned between ethyl acetate and water and the organic layer was separated, washed with water, dried (MgSO4) and evaporated to a white foam; purification by preparative t.l.c. (ethyl acetate: benzene 1:2.5) gave the title compound (510mg.), m.p. 140° dec.; [α]D + 133° (c 0.95).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US03983111 |
| Source dataset | uspto-grants-1976_09 |
| ORD ID | ord-3b3bea7058c44df4a69d3924b0431d53 |
| Source note | uspto-grants-1976_09 |