HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tetrahydrofuran → HCID 67774375, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Isobutylene | HCID 8255 | — |
| Reactant | Sodium Chlorite | HCID 23668197 | — |
| Reactant | Monosodium phosphate | HCID 23672064 | — |
| Reactant | HCID 88415083 | HCID 88415083 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | tert-Butanol | HCID 6386 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Solvent | Sodium chloride; water | HCID 57417360 | — |
| Product | HCID 67774375 | HCID 67774375 | 98.1% |
Reaction Steps
The compound of step 7 (5.15 g, 11.42 mmol) was suspended in tert-butanol (90 ml), and a 2 M solution of isobutene in THF (34.27 ml, 68.53 mmol), a solution of sodium dihydrogenphosphate (4.111 g, 34.27 mmol) in 25 ml of water and sodium chlorite (1.937 g, 17.13 mmol) were added. The mixture was stirred at room temperature for 2 h. Then brine (200 ml), water (50 ml), EA (400 ml) and DCM (100 ml) were added and the organic phase was separated, dried over magnesium sulfate, filtered and evaporated to dryness. The obtained solid was triturated several times with cyclohexane and dried in vacuo at 50° C. 5.23 g of the title compound were obtained as a yellow solid melting at 193-194° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08415336B2 |
| Source dataset | uspto-grants-2013_04 |
| ORD ID | ord-cb9884dede1c403091f0651d580a27b1 |
| Source note | uspto-grants-2013_04 |