HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 11581759, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Reactant | HCID 22225349 | HCID 22225349 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Diisopropylethylamine | HCID 81531 | — |
| Product | HCID 11581759 | HCID 11581759 | 71% |
Reaction Steps
A mixture of compound H (19 g; 0.04423 mol) and DBU (14 mL; 0.0936) in 110 mL of N,N-diisopropylethylamine and 30 mL of THF was refluxed for 30 h. The reaction mixture was poured into 600 mL of iced water and extracted with ethyl acetate (3×500 mL). The organic phase was washed with water and brine, dried over anhydrous sodium sulphate and concentrated. The crude was purified by silica gel column chromatography (eluant: n-hexane/ethyl acetate=2/1 to 1/2) to yield compound 1 (12 g; 71%) as a yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07019002B2 |
| Source dataset | uspto-grants-2006_03 |
| ORD ID | ord-e45c06741a074ea2a72181b3f3469b20 |
| Source note | uspto-grants-2006_03 |