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

HRID 1862926ノート

反応式

HRID 1862926 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a7f8f168974f43b487ec7b1539632e9d
出典データセット
uspto-grants-1979_09
特許番号
US04166813

反応ノート

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