HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tributylphosphine → HCID 66648457, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tributylphosphine | HCID 13831 | — |
| Reactant | 1,1'-(Azodicarbonyl)dipiperidine | HCID 73042 | — |
| Reactant | tert-butyl N-(2-hydroxyethyl)carbamate | HCID 2733206 | — |
| Reactant | HCID 59706557 | HCID 59706557 | — |
| Solvent | Benzene | HCID 241 | — |
| Product | HCID 66648457 | HCID 66648457 | 98% |
Reaction Steps
To a solution of 2-(4-hydroxybenzyl)-3-isopropylmaleic acid dimethyl ester (204.5 mg, 0.6996 mmol) in benzene (6 mL) were added N-(t-butoxycarbonyl)ethanolamine (343 mg, 2.13 mol), tributylphosphine (853 mg, 4.20 mmol) and 1,1′-(azodicarbonyl)dipiperidine (1.05 g, 4.20 mmol) with stirring at room temperature. After stirring at room temperature for 1 h, the reaction mixture was filtered, and the residue obtained by concentrating the filtrate under reduced pressure was subjected to silica gel column chromatography (hexane-ethyl acetate 2:1) to give 287 mg of dimethyl 2-{4-[2-(t-butoxycarbonylamino)ethoxy]benzyl}-3-isopropylmaleate as oil (yield: 98%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09260375B2 |
| Source dataset | uspto-grants-2016_02 |
| ORD ID | ord-c5420720e2c04db99c0f33b58ccd9d26 |
| Source note | uspto-grants-2016_02 |