Potassium Carbonate → alpha-Ethyl-alpha-(4-chlorophenyl)-4-[3-(di-n-propylamino)-propoxy]-benzylalcohol

HRID 236568ノート

反応式

HRID 236568 の反応式
[CH2:1]([C:3]([OH:18])([C:11]1[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][CH:12]=1)[C:4]1[CH:9]=[CH:8][C:7]([OH:10])=[CH:6][CH:5]=1)[CH3:2].C(=O)([O-])[O-].[K+].[K+].[CH2:25]([N:28]([CH2:32][CH2:33][CH2:34]Cl)[CH2:29][CH2:30][CH3:31])[CH2:26][CH3:27]>S([O-])(O)(=O)=O.C([N+](CCCC)(CCCC)CCCC)CCC.C(OCC)(=O)C>[CH2:1]([C:3]([OH:18])([C:11]1[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][CH:12]=1)[C:4]1[CH:5]=[CH:6][C:7]([O:10][CH2:27][CH2:26][CH2:25][N:28]([CH2:32][CH2:33][CH3:34])[CH2:29][CH2:30][CH3:31])=[CH:8][CH:9]=1)[CH3:2]

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 12333917Dipropylaminopropyl chlorideHCID 14727318alpha-Ethyl-alpha-(4-chlorophenyl)-4-hydroxy-benzylalcohol

生成物 1

HCID 20216260alpha-Ethyl-alpha-(4-chlorophenyl)-4-[3-(di-n-propylamino)-propoxy]-benzylalcohol

試薬・触媒・溶媒 2

HCID 94433Tetrabutylammonium hydrogen sulfate触媒HCID 8857Ethyl Acetate溶媒

実験手順

13.1 g. of α-ethyl-α-(4-chlorophenyl)-4-hydroxy-benzylalcohol, 14 g. of anhydrous potassium carbonate, 9.8 g. of dipropylaminopropyl chloride and 0.85 g. of tetrabutyl ammonium hydrogensulfate in 135 ml. of ethyl acetate are slightly boiled for 20 hours, under stirring. After cooling the mixture, the solvent is evaporated in vacuo. To the residue water and benzene are added. The phases are separated, the benzene solution is washed with water, dried over anhydrous potassium carbonate, filtered and evaporated. The residue is purified by vacuum fractionation. 13.8 g. of the desired end product are obtained, boiling at 198° to 200° C./1.33 Pa.

後処理

  1. temperatureAfter cooling the mixture
  2. customthe solvent is evaporated in vacuo
  3. additionTo the residue water and benzene are added
  4. customThe phases are separated
  5. washthe benzene solution is washed with water
  6. dry with materialdried over anhydrous potassium carbonate
  7. filtrationfiltered
  8. customevaporated
  9. customThe residue is purified by vacuum fractionation
  10. customof the desired end product are obtained

出典と根拠

ORDレコード
ord-207e32b5a3714d40af02fe0ad4959c98
出典データセット
uspto-grants-1987_02
特許番号
US04645779

反応ノート

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