HRID1759229

反应详情

EQUATION

反应方程式

HRID 1759229 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a cooled solution of 7-(1-benzyloxycarbonyl-1-azidomethyl)-3-phenoxymethyl-6-oxo-2-thia-4,7-diazabicyclo[3,2,0]hept-3-ene (3.0 g.) in tetrahydrofuran (48 ml.) was added silver tetrafluoroborate (2.05 g.), followed by a solution of p-toluenesulfonic acid (145.8 mg.) in water (8.1 ml.). After the resultant mixture was stirred at 0° C. for 9 hours, it was concentrated to a volume of 10 ml. To the concentrate was added a mixture of methanol (5 ml.) and water (10 ml.) and precipitates were triturated, filtered and washed with water (three times), a mixture of methanol (5 ml.) and water (10 ml.) (several times), methanol, diethyl ether and hexane, successively to give silver salt at the mercapto group of benzyl 2-azido-2-(3-phenoxyacetamido-4-mercapto-2-oxo-1-azetidinyl)acetate (3.75 g.).

WORKUP

后处理

  1. concentrationit was concentrated to a volume of 10 ml
  2. additionTo the concentrate was added
  3. additiona mixture of methanol (5 ml.) and water (10 ml.)
  4. customprecipitates
  5. customwere triturated
  6. filtrationfiltered
  7. washwashed with water (three times)
  8. additiona mixture of methanol (5 ml.) and water (10 ml.) (several times), methanol, diethyl ether and hexane