Hydrochloric Acid → diethyl 3-(N-ethoxycarbonyl-N-ethoxycarbonyloxyamino)-2-hydroxypropylphosphonate
반응식
[CH2:1]([O:3][C:4]([N:6]([CH2:13][CH:14]([O:24]C1CCCCO1)[CH2:15][P:16](=[O:23])([O:20][CH2:21][CH3:22])[O:17][CH2:18][CH3:19])[O:7][C:8]([O:10][CH2:11][CH3:12])=[O:9])=[O:5])[CH3:2].Cl>C(O)C>[CH2:1]([O:3][C:4]([N:6]([CH2:13][CH:14]([OH:24])[CH2:15][P:16](=[O:23])([O:20][CH2:21][CH3:22])[O:17][CH2:18][CH3:19])[O:7][C:8]([O:10][CH2:11][CH3:12])=[O:9])=[O:5])[CH3:2]참가 물질
4
실험 절차
A mixture of diethyl 3-(N-ethoxycarbonyl-N-ethoxycarbonyloxyamino)-2-(tetrahydro-2H-pyran-2-yloxy)propylphosphonate (54.0 g.), ethanol (100 ml.) and 0.1 N hydrochloric acid (100 ml.) was stirred for 4 hours at ambient temperature. After the reaction was completed, the ethanol was distilled off from the reaction mixture under reduced pressure to give an aqueous solution, which was extracted three times with ethyl acetate (200 ml. once and 50 ml. twice). The combined extracts were washed with a saturated sodium chloride aqueous solution, dried over magnesium sulfate, and evaporated to dryness under reduced pressure to give oily diethyl 3-(N-ethoxycarbonyl-N-ethoxycarbonyloxyamino)-2-hydroxypropylphosphonate (39.25 g.).
후처리
- distillationthe ethanol was distilled off from the reaction mixture under reduced pressure
- customto give an aqueous solution, which
- extractionwas extracted three times with ethyl acetate (200 ml
- washThe combined extracts were washed with a saturated sodium chloride aqueous solution
- dry with materialdried over magnesium sulfate
- customevaporated to dryness under reduced pressure
출처 및 근거
- ORD 기록
- ord-55475f92675e4566853a9601f4dec8af
- 출처 데이터셋
- uspto-grants-1980_01
- 특허 번호
- US04182758
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