Phenyl isocyanate → Bis{3-[N-butyl-N-(2,2,6,6-tetramethyl-4-piperidyl)amino]-2-phenylcarbamoyloxypropyl}1,2-cyclohexanedicarboxylate

HRID 1862926노트

반응식

HRID 1862926 반응식
[CH2:1]([N:5]([CH2:16][CH:17]([OH:50])[CH2:18][O:19][C:20]([CH:22]1[CH2:27][CH2:26][CH2:25][CH2:24][CH:23]1[C:28]([O:30][CH2:31][CH:32]([OH:49])[CH2:33][N:34]([CH2:45][CH2:46][CH2:47][CH3:48])[CH:35]1[CH2:40][C:39]([CH3:42])([CH3:41])[NH:38][C:37]([CH3:44])([CH3:43])[CH2:36]1)=[O:29])=[O:21])[CH:6]1[CH2:11][C:10]([CH3:13])([CH3:12])[NH:9][C:8]([CH3:15])([CH3:14])[CH2:7]1)[CH2:2][CH2:3][CH3:4].[C:51]1([N:57]=[C:58]=[O:59])[CH:56]=[CH:55][CH:54]=[CH:53][CH:52]=1>C1C=CC=CC=1>[CH2:1]([N:5]([CH2:16][CH:17]([O:50][C:58](=[O:59])[NH:57][C:51]1[CH:56]=[CH:55][CH:54]=[CH:53][CH:52]=1)[CH2:18][O:19][C:20]([CH:22]1[CH2:27][CH2:26][CH2:25][CH2:24][CH:23]1[C:28]([O:30][CH2:31][CH:32]([O:49][C:58](=[O:59])[NH:57][C:51]1[CH:56]=[CH:55][CH:54]=[CH:53][CH:52]=1)[CH2:33][N:34]([CH2:45][CH2:46][CH2:47][CH3:48])[CH:35]1[CH2:40][C:39]([CH3:42])([CH3:41])[NH:38][C:37]([CH3:44])([CH3:43])[CH2:36]1)=[O:29])=[O:21])[CH:6]1[CH2:11][C:10]([CH3:13])([CH3:12])[NH:9][C:8]([CH3:14])([CH3:15])[CH2:7]1)[CH2:2][CH2:3][CH3:4]

참가 물질

4

반응물 2

HCID 7672Phenyl isocyanateHCID 86736634Bis{3-[N-butyl-N-(2,2,6,6-tetramethyl-4-piperidyl)amino]-2-hydroxypropyl}1,2-cyclohexanedicarboxylate

생성물 1

HCID 86736635Bis{3-[N-butyl-N-(2,2,6,6-tetramethyl-4-piperidyl)amino]-2-phenylcarbamoyloxypropyl}1,2-cyclohexanedicarboxylate

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

A mixture of 2.4 g of bis{3-[N-butyl-N-(2,2,6,6-tetramethyl-4-piperidyl)amino]-2-hydroxypropyl}1,2-cyclohexanedicarboxylate, obtained as described in Example 18, and 2.4 g of phenylisocyanate in 30 ml of benzene was refluxed, with stirring, for 3 hours. At the end of this time, the solvent was removed from the reaction mixture by evaporation under reduced pressure and the resulting residue was purified by column chromatography through silica gel eluted with a 20:1 by volume mixture of ethyl acetate and triethylamine. The desired compound was obtained in the form of a vitreous mass having an Rf value of 0.58 on thin layer chromatography on silica gel developed with a 5:1 by volume mixture of ethyl acetate and triethylamine.

후처리

  1. customobtained
  2. temperaturewas refluxed
  3. customAt the end of this time, the solvent was removed from the reaction mixture by evaporation under reduced pressure
  4. customthe resulting residue was purified by column chromatography through silica gel
  5. washeluted with a 20:1 by volume mixture of ethyl acetate and triethylamine

출처 및 근거

ORD 기록
ord-a7f8f168974f43b487ec7b1539632e9d
출처 데이터셋
uspto-grants-1979_09
특허 번호
US04166813

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