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

HRID 1706183ノート

反応式

HRID 1706183 の反応式
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]

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒2 回

実験手順

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 soluion 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.).

後処理

  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 soluion saturated with sodium chloride
  7. dry with materialdried over magnesium sulfate
  8. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-65d40dba730e4e6c82fc3948f60ab1e4
出典データセット
uspto-grants-1980_06
特許番号
US04206156

反応ノート

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