반응 #595346
ord-a7fa4604d7d7428d90a722e1774742b3
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시약
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후처리
- 1workup.ADDITIONAfter the addition
- 2온도the reaction solution is slowly warmed to RT
- 3workup.STIRRINGWith stirring
- 4온도the mixture is then heated
- 5온도at reflux for 2 h
- 6온도The mixture is then cooled again to 0° C.
- 7workup.STIRRINGthe mixture is stirred at RT for 3 h
- 8기타The precipitate formed
- 9여과is filtered off
- 10기타the filtrate is freed from the solvent on a rotary evaporator
- 11기타The residue is used without further purification in the subsequent reaction
실험 절차
166 mg (4.38 mmol) of lithium aluminum hydride are initially charged in 10 ml of dry THF and cooled to 0° C. A solution of 260 mg (1.09 mmol) of the compound from Example 37A in 10 ml of dry THF is added dropwise. After the addition has ended, the reaction solution is slowly warmed to RT and stirred at this temperature for 1 h. With stirring, the mixture is then heated at reflux for 2 h. The mixture is then cooled again to 0° C., 0.4 ml of water and 0.8 ml of 1 N aqueous sodium hydroxide solution are added carefully and the mixture is stirred at RT for 3 h. The precipitate formed is filtered off, and the filtrate is freed from the solvent on a rotary evaporator. The residue is used without further purification in the subsequent reaction.