반응 #93176

ord-bf3ac941a9f04771a1236503f1887025

반응 방정식

O=B[O-].[Na+]
sodium boranate
C=CCOc1ccc(OC(C(=O)C(C)(C)C)n2cncn2)cc1
1-(4-allyloxyphenoxy)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)-2-butanone
C=CCOc1ccc(OC(C(O)C(C)(C)C)n2cncn2)cc1
1-(4-allyloxyphenoxy)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)-2-butanol
수율 97.2%

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.STIRRINGThe mixture is subsequently stirred for 1 hour
  2. 2
    농축is then concentrated in vacuo
  3. 3
    workup.DISTILLATIONby distilling off the solvent
  4. 4
    기타The residue is partitioned between methylene chloride and water
  5. 5
    기타The organic phase is separated off
  6. 6
    건조dried over sodium sulphate
  7. 7
    농축concentrated in vacuo

실험 절차

1 g (0.027 mole) of sodium boranate is added in portions to 7.2 g (0.023 mole) of 1-(4-allyloxyphenoxy)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)-2-butanone (Example 1) in 80 ml of methanol at 20° C., while stirring. The mixture is subsequently stirred for 1 hour and is then concentrated in vacuo by distilling off the solvent. The residue is partitioned between methylene chloride and water. The organic phase is separated off, dried over sodium sulphate and concentrated in vacuo. 7 g (97.2% of theory) of 1-(4-allyloxyphenoxy)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)-2-butanol of melting point 85° C. are obtained.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04610996uspto-grants-1986_09