HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 131721737, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Lithium borohydride | HCID 4148881 | — |
| Reactant | HCID 131721736 | HCID 131721736 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 131721737 | HCID 131721737 | 48.4% |
Reaction Steps
To a suspension of the compound (100 mg) obtained in Example 157 in anhydrous tetrahydrofuran (THF; 20 ml) was added lithium borohydride (5.5 mg) under cooling with ice. The mixture was stirred for 5 minutes. After adding another lithium borohydride (5.5 mg), the mixture was stirred for further 5 minutes. Water was added to the reaction mixture, followed by extraction with methylene chloride. The organic layer was washed with saturated aqueous solution of sodium chloride and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure and the residue was purified by silica gel column chromatography (ethyl acetate/methylene chloride=1:1) to yield 45 mg (48%) of the titled compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06040331 |
| Source dataset | uspto-grants-2000_03 |
| ORD ID | ord-edc979f4063847bcb5279232fd2a0d11 |
| Source note | uspto-grants-2000_03 |