反应 #59271

ord-50155863f6ec4ac090cace69e4b37baf

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他the phases separated
  2. 2
    萃取After extraction of the organic phases with water (5 ml) and saturated aqueous sodium chloride (5 ml)
  3. 3
    干燥the solution is dried with magnesium sulfate
  4. 4
    其他evaporated to dryness
  5. 5
    其他MS: m/e=297(M+H+), which was used without further purification

实验过程

((S)-7-tert-Butoxycarbonylamino-6-oxo-6,7-dihydro-dibenzo[b,d]azepin-5-yl)-acetic acid methyl ester (60 mg, 0.15 mmol) were dissolved in dichloromethane (3 ml), treated with 0.15 ml (2.3 mmol) orthophosphoric acid and stirred for 18 .h The reaction mixture is adjusted to pH 7.5 with 2N aqueous sodium hydroxide, diluted with dichloromethane (5 ml) and the phases separated. After extraction of the organic phases with water (5 ml) and saturated aqueous sodium chloride (5 ml), the solution is dried with magnesium sulfate and evaporated to dryness. White solid (60%); MS: m/e=297(M+H+), which was used without further purification.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07425551B2uspto-grants-2008_09