HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl isocyanate → HCID 69550224, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl isocyanate | HCID 8022 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 10234018 | HCID 10234018 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 69550224 | HCID 69550224 | — |
Reaction Steps
To a stirred solution of N-(1-{[1-sec-butyl-4-(2-{2-[2-(3-hydroxy-phenyl)-ethylcarbamoyl]-1-methylsulfanyl-propyl}-pyrrolidin-1-yl)-2-methoxy-4-oxo-butyl]-methyl-carbamoyl}-2-methyl-propyl)-2-dimethylamino-3-methyl-butyramide (30 mg, 0.035 mmol) in CH2Cl2 (0.5 mL) were added ethyl isocyanate (0.042 mL, 0.53 mmol) and diisopropylethylamine (0.062 mL, 0.35 mmol) at room temperature. After being stirred at room temperature for 13hr, the mixture was concentrated in vacuo to give a crude oil (58 mg), which was purified by preparative HPLC (column:ODS-8OTs, eluent: 35/35 H2O:CH3CN/0.05% TFA). The appropriate fractions were lyophilized to give the title compound as a white amorphous powder (13 mg, 39%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06737409B2 |
| Source dataset | uspto-grants-2004_05 |
| ORD ID | ord-5ac4a5b6d1854aae989f29d763255330 |
| Source note | uspto-grants-2004_05 |