Cyclohexylamine → decyl N-trifluoroacetyl-N-(bis(cyclohexylamino)phosphonomethyl)glycinate

HRID 2413069

反応式

HRID 2413069 の反応式
[F:1][C:2]([F:28])([F:27])[C:3]([N:5]([CH2:20][P:21]([O:25]Cl)([O:23]Cl)=[O:22])[CH2:6][C:7]([O:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19])=[O:8])=[O:4].[CH:29]1([NH2:35])[CH2:34][CH2:33][CH2:32][CH2:31][CH2:30]1>CCOCC>[F:1][C:2]([F:28])([F:27])[C:3]([N:5]([CH2:20][P:21]([O:25][NH:35][CH:29]1[CH2:34][CH2:33][CH2:32][CH2:31][CH2:30]1)([O:23][NH:35][CH:29]1[CH2:34][CH2:33][CH2:32][CH2:31][CH2:30]1)=[O:22])[CH2:6][C:7]([O:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19])=[O:8])=[O:4]

参加物

4

反応物 2

HCID 7965CyclohexylamineHCID 53672523decyl N-trifluoroacetyl-N-(dichlorophosphonomethyl)glycinate

生成物 1

HCID 54141188decyl N-trifluoroacetyl-N-(bis(cyclohexylamino)phosphonomethyl)glycinate

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

To a solution of decyl N-trifluoroacetyl-N-(dichlorophosphonomethyl)glycinate (6.63 g, 0.015 mole) in 200 ml. of ether was added with good stirring cyclohexylamine (5.95 g, 0.06 mole) in 50 ml. of ether. The reaction was stirred overnight at room temperature, then filtered, and the filtrate concentrated in vacuo. The residue was dissolved in fresh ether, washed with water, dried over MgSO4 and concentrated in vacuo. The residue was eluted through a dry column chromatograph with ethyl acetate to yield decyl N-trifluoroacetyl-N-(bis(cyclohexylamino)phosphonomethyl)glycinate, m.p. 79.5°-82.5° C.

後処理

  1. filtrationfiltered
  2. concentrationthe filtrate concentrated in vacuo
  3. dissolutionThe residue was dissolved in fresh ether
  4. washwashed with water
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated in vacuo
  7. washThe residue was eluted through a dry column chromatograph with ethyl acetate

出典と根拠

ORDレコード
ord-25ff4916de9e495282149876b7093c2f
出典データセット
uspto-grants-1985_01
特許番号
US04496389

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