Hydrochloric Acid → diethyl 3-(N-ethoxycarbonyl-N-ethoxycarbonyloxyamino)-2-hydroxypropylphosphonate
反応式
[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]参加物
4
実験手順
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.).
後処理
- 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
出典と根拠
- ORDレコード
- ord-d0359736582f4862aa085d9391d4ab13
- 出典データセット
- uspto-grants-1980_06
- 特許番号
- US04206156
反応ノート
読み込み中…