1-Butanol → HCID 20510602、化合物

HRID 1758193ノート

反応式

HRID 1758193 の反応式
C(O)[CH2:2][CH2:3][CH3:4].[OH:6][CH2:7][CH:8]1[CH2:12][O:11][C:10]2([CH2:17][C:16]([CH3:19])([CH3:18])[NH:15][C:14]([CH3:21])([CH3:20])[CH2:13]2)[O:9]1.[O:22]1[CH2:46][CH:23]1[CH2:24][O:25][C:26]1[CH:31]=[CH:30][C:29]([C:32]([C:35]2[CH:40]=[CH:39][C:38]([O:41][CH2:42][CH:43]3[O:45][CH2:44]3)=[CH:37][CH:36]=2)([CH3:34])[CH3:33])=[CH:28][CH:27]=1.[C:47]([O:50][CH2:51][CH3:52])(=[O:49])[CH3:48].[CH2:53]([OH:55])C>C(N(CC)CC)C>[OH:45][CH:43]([CH2:44][N:15]1[C:14]([CH3:21])([CH3:20])[CH2:13][C:47]2([O:49][CH:52]([CH2:53][OH:55])[CH2:51][O:50]2)[CH2:48][C:3]1([CH3:2])[CH3:4])[CH2:42][O:41][C:38]1[CH:39]=[CH:40][C:35]([C:32]([C:29]2[CH:30]=[CH:31][C:26]([O:25][CH2:24][CH:23]([OH:22])[CH2:46][N:15]3[C:14]([CH3:21])([CH3:20])[CH2:13][C:10]4([O:9][CH:8]([CH2:7][OH:6])[CH2:12][O:11]4)[CH2:17][C:16]3([CH3:19])[CH3:18])=[CH:27][CH:28]=2)([CH3:34])[CH3:33])=[CH:36][CH:37]=1

参加物

7

反応物 5

HCID 2631-ButanolHCID 702EthanolHCID 2286Bisphenol A diglycidyl etherHCID 8857Ethyl AcetateHCID 50162607,7,9,9-TETRAMETHYL-1,4-DIOXA-8-AZASPIRO[4.5]DECANE-2-METHANOL

生成物 1

HCID 20510602HCID 20510602、化合物

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

To 80 ml of n-butanol were added 10.0 g of 2-hydroxymethyl-7,7,9,9-tetramethyl-1,4-dioxa-8-azaspiro[4.5]decane and 6.2 g of 2,2-bis[p-(2,3-epoxypropoxy)phenyl]propane and the mixture was refluxed for 3 days. After completion of the reaction, the solvent was removed from the reaction mixture by evaporation under reduced pressure and ethyl acetate was added to the residue. The ethyl acetate solution was washed with water and dried over anhydrous magnesium sulphate. The residue obtained by removing the solvent, by evaporation under reduced pressure, from the ethyl acetate solution was purified by column chromatography through silica gel eluted with a 20:1:1 by volume mixture of ethyl acetate, ethanol and triethylamine. The desired Compound No. 161 was obtained in the form of a vitreous solid having an Rf value of 0.45 on thin-layer chromatography on silica gel developed with a 20:1:1 by volume mixture of ethyl acetate, ethanol and triethylamine.

後処理

  1. temperaturethe mixture was refluxed for 3 days
  2. customAfter completion of the reaction
  3. customthe solvent was removed from the reaction mixture by evaporation under reduced pressure and ethyl acetate
  4. additionwas added to the residue
  5. washThe ethyl acetate solution was washed with water
  6. dry with materialdried over anhydrous magnesium sulphate
  7. customThe residue obtained
  8. customby removing the solvent
  9. customby evaporation under reduced pressure
  10. customfrom the ethyl acetate solution was purified by column chromatography through silica gel
  11. washeluted with a 20:1:1 by volume mixture of ethyl acetate, ethanol and triethylamine
  12. custom161 was obtained in the form of a vitreous solid

出典と根拠

ORDレコード
ord-57a8f25bbb954a10aad3ede7f118afe5
出典データセット
uspto-grants-1983_02
特許番号
US04371644

反応ノート

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