반응 #790926

ord-359b51b9ed884268b1bbd3fb2f630341

반응 방정식

[K+].[OH-]
potassium hydroxide
OCCO
ethylene glycol
O=[N+]([O-])c1ccc2c(c1)OCO2
3,4-methylenedioxynitrobenzene
CC(O)Oc1ccc([N+](=O)[O-])cc1O
2-hydroxy-4-nitrophenoxyethanol

반응 조건

온도
-5°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타being kept in the region of 100° C
  2. 2
    온도After heating for two hours
  3. 3
    기타The expected product crystallizes in the form of the potassium phenate
  4. 4
    여과The phenate is filtered off
  5. 5
    workup.DISSOLUTIONredissolved in 250 ml of water
  6. 6
    기타The 2-hydroxy-4-nitrophenoxyethanol precipitates
  7. 7
    여과After filtration
  8. 8
    세척washing with water
  9. 9
    기타drying in vacuo

실험 절차

0.2 mol (11.2 g) of potassium hydroxide is dissolved in 167 ml of ethylene glycol in a boiling water bath. 0.1 mol (16.7 g) of 3,4-methylenedioxynitrobenzene is added, with stirring, the temperature being kept in the region of 100° C. After heating for two hours, the reaction medium is cooled to -5° C. The expected product crystallizes in the form of the potassium phenate. The phenate is filtered off and then redissolved in 250 ml of water, and the solution is acidified to pH=6 with concentrated hydrochloric acid. The 2-hydroxy-4-nitrophenoxyethanol precipitates. After filtration, washing with water and drying in vacuo, the expected product melts at 158° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04985042uspto-grants-1991_01