HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 68527763, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 131729319 | HCID 131729319 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 68527763 | HCID 68527763 | 45.1% |
Reaction Steps
7.5 g (30 mmoles) of the product of Step 1 are dissolved in 15 mL of anhydrous tetrahydrofuran. The solution is poured dropwise into a suspension comprising 1.48 g (1.3 equivalents) of AlLiH4 suspended in 38 mL of anhydrous tetrahydrofuran. Stirring is carried out at 25° C. for 2 hours. The mixture is hydrolysed in the cold state using 2.7 mL of water, 2.7 mL of NaOH (20%) and then 2.7 mL of water. Filtration and evaporation of the filtrate to dryness are carried out. There are obtained 2.4 g of a residue which is purified by column chromatography over silica (eluant: CH2Cl2/ethanol/NH4OH: 95/5/0.5. The expected product is obtained in the form of a brown oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08076325B2 |
| Source dataset | uspto-grants-2011_12 |
| ORD ID | ord-815fb177dc53488fa3348f9ca4d0620c |
| Source note | uspto-grants-2011_12 |