반응 #595340

ord-1416c1ca9a0c43d886b805592fc7c512

반응 방정식

[Al+3].[H-].[H-].[H-].[H-].[Li+]
lithium aluminum hydride
CCOC(=O)c1coc(-c2ccc(Cl)c(C)c2)n1
compound
CCOC(=O)c1coc(-c2ccc(Cl)c(C)c2)n1
Ethyl 2-(4-chloro-3-methylphenyl)-1,3-oxazole-4-carboxylate
O
water
[Na+].[OH-]
sodium hydroxide
Cc1cc(-c2nc(CO)co2)ccc1Cl
[2-(4-Chloro-3-methylphenyl)-1,3-oxazol-4-yl]methanol

용매

반응 조건

온도
0°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The reaction solution is then once more cooled to 0° C.
  2. 2
    workup.STIRRINGThe mixture is stirred at RT overnight
  3. 3
    기타The precipitate formed
  4. 4
    여과is filtered off
  5. 5
    기타a rotary evaporator
  6. 6
    기타The residue is used without further purification in the subsequent reaction

실험 절차

46 mg (1.22 mmol) of lithium aluminum hydride are initially charged in 8.0 ml of THF and cooled to 0° C. A solution of 161 mg (0.61 mmol) of the compound from Example 26A in 2.5 ml of THF is then added dropwise. The mixture is stirred at RT for 2 h. The reaction solution is then once more cooled to 0° C., and 0.2 ml of water and 0.4 ml of 1 N aqueous sodium hydroxide solution are added. The mixture is stirred at RT overnight. The precipitate formed is filtered off, and the filtrate is freed from the solvent using a rotary evaporator. The residue is used without further purification in the subsequent reaction.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09095582B2uspto-grants-2015_08