반응 #3877

ord-f72db97d8ce54dbba8cafdb5ed72d91d

반응 방정식

CCOC(C)=O
ethyl acetate
O=C([O-])[O-].[K+].[K+]
potassium carbonate
CCOc1nnc(CBr)s1
2-bromomethyl-5-ethoxy-1,3,4-thiadiazole
Oc1ccc(Oc2ccccc2)cc1
4-phenoxy phenol
CCOC1=NN=C(Oc2ccc(Oc3ccccc3)cc2)[SH]1C
compound
수율 74.2%
CCOC1=NN=C(Oc2ccc(Oc3ccccc3)cc2)[SH]1C
2-ethoxy-5-[(4-phenoxy)phenoxy]-methyl-1,3,4-thiadiazole
수율 74.2%

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The resulting mixture was refluxed
  2. 2
    온도heated for 2 hours
  3. 3
    온도After cooling
  4. 4
    세척by washing with water for two times
  5. 5
    건조the resulting ethyl acetate layer was dried over anhydrous magnesium sulfate
  6. 6
    workup.DISTILLATIONEthyl acetate was distilled over under reduced pressure
  7. 7
    기타the residue was purified by chromatography on silica gel

실험 절차

0.76 g of 4-phenoxy phenol was dissolved in 10 ml of acetone followed by adding 0.6 g of anhydrous potassium carbonate and 1.0 g of 2-bromomethyl-5-ethoxy-1,3,4-thiadiazole. The resulting mixture was refluxed with stirring and heated for 2 hours. After cooling, 100 ml of ethyl acetate was added followed by washing with water for two times, and the resulting ethyl acetate layer was dried over anhydrous magnesium sulfate. Ethyl acetate was distilled over under reduced pressure, and the residue was purified by chromatography on silica gel to obtain 1.0 g of the compound No. 1 described in Table 1.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04722934uspto-grants-1988_02