HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetyl chloride → Methyl 7-hydroxyhept-5-ynoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 7-Acetoxy-hept-5-ynoic acid | HCID 21964419 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | Methyl 7-hydroxyhept-5-ynoate | HCID 11789443 | 92% |
Reaction Steps
The crude acid 29 (6.333 g) was treated with a 1% solution of acetyl chloride in methanol (60 mL). After 16 h, sodium bicarbonate (1.966 g, 23.4 mmol) was added. The mixture was dried (MgSO4), filtered through celite and evaporated in vacuo. Purification by flash chromatography on silica gel (30-40% ethyl acetate/hexanes) gave 7-Hydroxy-hept-5-ynoic acid methyl ester 30 (3.022 g, 19.3 mmol, 92% from 7-(tert-Butyl-dimethyl-silanyloxy)-hept-2-yn-1-ol 27).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09156810B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-1439f3b73b9d43bf87557976cd6044f5 |
| Source note | uspto-grants-2015_10 |