تفاعل #59271

ord-50155863f6ec4ac090cace69e4b37baf

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

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

الإجراء التجريبي

((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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07425551B2uspto-grants-2008_09