Hydrochloric Acid → diethyl 3-(N-ethoxycarbonyl-N-ethoxycarbonyloxyamino)-2-hydroxypropylphosphonate

HRID 2051976ノート

反応式

HRID 2051976 の反応式
[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

反応物 2

HCID 313Hydrochloric AcidHCID 20337196diethyl 3-(N-ethoxycarbonyl-N-ethoxycarbonyloxyamino)-2-(tetrahydro-2H-pyran-2-yloxy)propylphosphonate

生成物 1

HCID 20337198diethyl 3-(N-ethoxycarbonyl-N-ethoxycarbonyloxyamino)-2-hydroxypropylphosphonate収率 89.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

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

  1. distillationthe ethanol was distilled off from the reaction mixture under reduced pressure
  2. customto give an aqueous solution, which
  3. extractionwas extracted three times with ethyl acetate (200 ml
  4. washThe combined extracts were washed with a saturated sodium chloride aqueous solution
  5. dry with materialdried over magnesium sulfate
  6. customevaporated to dryness under reduced pressure

出典と根拠

ORDレコード
ord-55475f92675e4566853a9601f4dec8af
出典データセット
uspto-grants-1980_01
特許番号
US04182758

反応ノート

読み込み中…