HuagongsheHuagongshe Chemistry Print Report · For research reference only
3,5-Dihydroxybenzoic Acid → HCID 54533744, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3,5-Dihydroxybenzoic Acid | HCID 7424 | — |
| Reactant | Ethylmorpholine | HCID 7525 | — |
| Reactant | Dicyclohexylcarbodiimide | HCID 10868 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | Methyl tyrosinate hydrochloride | HCID 76956 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 54533744 | HCID 54533744 | — |
Reaction Steps
231.2 g of 3,5-dihydroxybenzoic acid are dissolved in 4 l of dimethyl formamide. 313 g of L-tyrosine-methyl ester hydrochloride, 202 g of 1-hydroxybenzotriazole and 346 ml of N-ethyl morpholine and subsequently 297 g of dicyclohexyl carbodiimide are added. The mixture is stirred over night at room temperature, and the precipitated dicyclohexyl urea is filtered off. The solvent is distilled off in vacuo, the residue is taken up in 4 l of ethyl acetate, the ethyl acetate solution is washed 4 times each with saturated sodium bicarbonate solution, 3 times with 400 ml portions of a solution of 5% KHSO4 and 10% K2SO4 and twice with 200 ml portions of water, dried over sodium sulfate and subsequently brought to dryness. Yield: 360 g of resin.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04302448 |
| Source dataset | uspto-grants-1981_11 |
| ORD ID | ord-59b1e071c50a4b51b292190f81ce430f |
| Source note | uspto-grants-1981_11 |