반응 #59271

반응 방정식

((S)-7-tert-Butoxycarbonylamino-6-oxo-6,7-dihydro-dibenzo[b,d]azepin-5-yl)-acetic acid methyl ester

orthophosphoric acid

sodium hydroxide

→

((S)-7-Amino-6-oxo-6,7-dihydro-dibenzo[b,d]azepin-5-yl)-acetic acid methyl ester

용매

dichloromethane

dichloromethane

반응 조건

후처리

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

실험 절차

((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.

출처