HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 46945368, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 2-Isocyanatobutane | HCID 550850 | — |
| Reactant | HCID 46945366 | HCID 46945366 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Product | HCID 46945368 | HCID 46945368 | 36% |
Reaction Steps
The compound of Example 25 (395 mg, 0.72 mmole) is dissolved in anhydrous 1,2-dichloroethane (10 ml) under an argon atmosphere, before the dropwise addition of sec-butylisocyanate (0.35 ml, 3 mmoles) at 23° C. The mixture is then heated under reflux for 24 hours. The reaction medium is then poured onto cold water and extracted using CH2Cl2. After decantation, the organic phase is washed with water and salt water. The organic solution is then dried over MgSO4, filtered, concentrated to dryness under vacuum and the evaporation residue is purified on a silica column (eluent: heptane/AcOEt: 1/0 to 4/6). The expected compound is obtained in the form of a colourless oil with a yield of 36%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08710091B2 |
| Source dataset | uspto-grants-2014_04 |
| ORD ID | ord-618c4242463042b18fcf5676750282e1 |
| Source note | uspto-grants-2014_04 |