HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 3beta-Caprylamido-7alpha,12alpha-dihydroxy-5beta-cholan-24-oic methylester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Hexanoyl chloride | HCID 67340 | — |
| Reactant | 3beta-amino-7alpha,12alpha-dihydroxy-5beta-cholan-24-oic Acid | HCID 54018831 | — |
| Product | 3beta-Caprylamido-7alpha,12alpha-dihydroxy-5beta-cholan-24-oic methylester | HCID 86585449 | — |
Reaction Steps
1.0 g of 3β-amino-7α,12α-dihydroxy-5β-cholan-24-oic Acid (FIG. 5A-15) methylester (FIG. 5A-1) [see Example I] was dissolved in 30 ml dry methylene chloride and treated with 15 ml triethyl amine under stirring. 1.2 g of caproyl chloride acid in 10 ml methylene chloride were added dropwise to the resulting solution, and the stirring was continued overnight. The reaction mixture was poured into water extracted with methylene chloride, the organic fraction was then dried over sodium sulfate, evaporated to dryness and chromatographed over silica gel with a mixture of ehtyl acetate and hexane (6:4 and 8:2), to give 0.7 g 3β-caprylamido-7α,12α-dihydroxy-5β-cholan-24-oic methylester (FIG. 5A-14)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06589946B2 |
| Source dataset | uspto-grants-2003_07 |
| ORD ID | ord-64d6d38e3663443cb3ee2b5169fcd9f1 |
| Source note | uspto-grants-2003_07 |