Water → HCID 57222029, compound
Reaction equation
[H-].[Al+3].[Li+].[H-].[H-].[H-].[F:7][C@H:8]([CH2:17][C@@H:18]([OH:23])[CH2:19][CH2:20][CH2:21][CH3:22])[CH2:9][C:10](OC(C)(C)C)=[O:11].O.[OH-].[Na+]>C1COCC1>[F:7][C@H:8]([CH2:17][C@@H:18]([OH:23])[CH2:19][CH2:20][CH2:21][CH3:22])[CH2:9][CH2:10][OH:11]Participants
6
Reactant 4
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 5 °C
Procedure
In a 100 ml flask were charged dried THF and 0.59 g of lithium aluminum hydride in a nitrogen stream, followed by cooling to 5° C. To the mixture was added dropwise a solution of 5.0 g of the compound obtained in Step 5 in 17 ml of dried THF over 20 minutes, followed by allowing the mixture to react at 35 to 40° C. for 3 hours. The reaction mixture was again cooled to 5° C., and a solution of 0.6 g of water and 2 ml of THF was added thereto over 30 minutes. Then, 1.6 ml of a 4% sodium hydroxide aqueous solution was added thereto, followed by stirring at that temperature for 1 hour.
Workup
- customto react at 35 to 40° C. for 3 hours
- temperatureThe reaction mixture was again cooled to 5° C.
Sources & evidence
- ORD record
- ord-4f81090b4d74455ea58b81ef78df7f4a
- Source dataset
- uspto-grants-2000_07
- Patent number
- US06093345
Reaction notes
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