HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ingenol → (4S,5R,6R,18R)-4,5-dihydroxy-3,8,8,15,15,18-hexamethyl-7,9-dioxapentacyclo[11.5.1.01,5.06,11.014,16]nonadeca-2,11-dien-19-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ingenol | HCID 442042 | — |
| Reactant | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| Solvent | Acetone | HCID 180 | — |
| Product | (4S,5R,6R,18R)-4,5-dihydroxy-3,8,8,15,15,18-hexamethyl-7,9-dioxapentacyclo[11.5.1.01,5.06,11.014,16]nonadeca-2,11-dien-19-one | HCID 91827745 | — |
Reaction Steps
Ingenol is reacted with p-toluenesulphonic acid hydrate and acetone to give ingenol-5,20-acetonide according to the procedure of Opferkuch et al. (1981). Ingenol-5,20-acetonide is converted to the ingenol 3-acylate by treatment with the appropriate acyl chloride and 4-(N,N-dimethylamino)pyridine or pyridine in toluene or benzene, or treatment with the appropriate acid, an alkylpyridinium salt and tributylamine in toluene then treatment with methanolic perchloric acid according to the procedure of Sorg et al. (1982). The ingenol 3-acylate could be converted to the 20-chloro-20-deoxyingenol 3-acylate 5-benzoate by the method of Example 15.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07378445B2 |
| Source dataset | uspto-grants-2008_05 |
| ORD ID | ord-74b874e03e8946aeac0449164807c659 |
| Source note | uspto-grants-2008_05 |