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

HRID 223310

반응식

HRID 223310 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-d89c3f19fa344c25a73dac7a99ef371b
출처 데이터셋
uspto-grants-1982_10
특허 번호
US04353731

연결된 노트

불러오는 중…