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

HRID 2198672

반응식

HRID 2198672 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-573c2c82739e49998a8a19df80984856
출처 데이터셋
uspto-grants-1982_11
특허 번호
US04359332

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