Dimethylformamide → diethyl 3-(N-ethoxycarbonyl-N-ethoxycarbonyloxyamino)-2-methylpropylphosphonate

HRID 2051973노트

반응식

HRID 2051973 반응식
Cl[CH2:2][CH:3]([CH3:13])[CH2:4][P:5](=[O:12])([O:9][CH2:10][CH3:11])[O:6][CH2:7][CH3:8].[K].[CH2:15]([O:17][C:18]([O:20][NH:21][C:22](=[O:26])[O:23][CH2:24][CH3:25])=[O:19])[CH3:16].CN(C)C=O>C(OCC)(=O)C.O>[CH2:24]([O:23][C:22]([N:21]([CH2:2][CH:3]([CH3:13])[CH2:4][P:5](=[O:12])([O:9][CH2:10][CH3:11])[O:6][CH2:7][CH3:8])[O:20][C:18]([O:17][CH2:15][CH3:16])=[O:19])=[O:26])[CH3:25]

참가 물질

7

반응물 4

HCID 6228DimethylformamideHCID 5462222PotassiumHCID 11446651Ethyl EthoxycarbonyloxycarbamateHCID 20337215Diethyl 3-chloro-2-methylpropylphosphonate

생성물 1

HCID 20337240diethyl 3-(N-ethoxycarbonyl-N-ethoxycarbonyloxyamino)-2-methylpropylphosphonate수율 82%

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매2회

실험 절차

A mixture of diethyl 3-chloro-2-methylpropylphosphonate (22.8 g.), potassium salt of ethyl N-ethoxycarbonyloxycarbamate (21.5 g.) and dry N,N-dimethylformamide (114 ml.) was stirred at 80°-85° C. for 3 hours and then concentrated under reduced pressure to give an oily residue, to which was added a mixture of water (100 ml.) and ethyl acetate (100 ml.) The ethyl acetate layer was separated and the resultant aqueous layer was saturated with sodium chloride and extracted again with ethyl acetate (50 ml.). The combined ethyl acetate layer was washed with aqueous solution saturated with sodium chloride, dried over magnesium sulfate and concentrated under reduced pressure to give oily diethyl 3-(N-ethoxycarbonyl-N-ethoxycarbonyloxyamino)-2-methylpropylphosphonate (30.2 g.).

후처리

  1. concentrationconcentrated under reduced pressure
  2. customto give an oily residue
  3. additionto which was added
  4. customwas separated
  5. extractionextracted again with ethyl acetate (50 ml.)
  6. washThe combined ethyl acetate layer was washed with aqueous solution saturated with sodium chloride
  7. dry with materialdried over magnesium sulfate
  8. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-a50c96582fd049d3b5b4ffb88558c614
출처 데이터셋
uspto-grants-1980_01
특허 번호
US04182758

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