Water → N-[4-[[2-Hydroxy-3-[4-(2-methoxyethyl)phenoxy]propyl]aminomethyl]phenyl]methanesulfonamide hydrochloride

HRID 728825ノート

反応式

HRID 728825 の反応式
[O:1]1[CH:3]([CH2:4][O:5][C:6]2[CH:11]=[CH:10][C:9]([CH2:12][CH2:13][O:14][CH3:15])=[CH:8][CH:7]=2)[CH2:2]1.[ClH:16].[NH2:17][CH2:18][C:19]1[CH:24]=[CH:23][C:22]([NH:25][S:26]([CH3:29])(=[O:28])=[O:27])=[CH:21][CH:20]=1.O>CON[C@H](C(O)=O)CC1N=CNC=1.[OH-].[K+].CO>[ClH:16].[OH:1][CH:3]([CH2:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([CH2:12][CH2:13][O:14][CH3:15])=[CH:8][CH:7]=1)[CH2:2][NH:17][CH2:18][C:19]1[CH:20]=[CH:21][C:22]([NH:25][S:26]([CH3:29])(=[O:28])=[O:27])=[CH:23][CH:24]=1

参加物

7

反応物 3

HCID 962WaterHCID 92515((p-(2-Methoxyethyl)phenoxy)methyl)oxiraneHCID 27609964-(Methylsulfonylamino)benzylamine hydrochloride

生成物 1

HCID 67689935N-[4-[[2-Hydroxy-3-[4-(2-methoxyethyl)phenoxy]propyl]aminomethyl]phenyl]methanesulfonamide hydrochloride

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 14797Potassium Hydroxide溶媒HCID 178502851MeOHis溶媒

実験手順

1,2-epoxy-3-[4-(2-methoxyethyl)phenoxy]propane (63.7 mmol) in 15 mL of MeOHis added dropwise to a solution of N-[4-(aminomethyl)phenyl]methanesulfonamide hydrochloride (62.4 mmol) in 1M KOH in MeOH (65 mL) at room temperature. H2O (5 mL) is added ad the mixture is refluxed overnight. Methanol is removed from the cooled mixture under reduced pressure, and the residue is partitioned between H2O and CH2Cl2, and the combined organic portions are washed with brine and dried with anhydrous Na2SO4. After removal of the solvent under reduced pressure the hydrochloride salt is formed and recrystallized with CH3CN/MeOH to yield the title compound.

後処理

  1. temperatureis refluxed overnight
  2. customMethanol is removed from the cooled mixture under reduced pressure
  3. customthe residue is partitioned between H2O and CH2Cl2
  4. washthe combined organic portions are washed with brine
  5. dry with materialdried with anhydrous Na2SO4
  6. customAfter removal of the solvent under reduced pressure the hydrochloride salt
  7. customis formed
  8. customrecrystallized with CH3CN/MeOH

出典と根拠

ORDレコード
ord-5c31cd1d8aa349ea9f35a71853cf0cf4
出典データセット
uspto-grants-1991_09
特許番号
US05051423

反応ノート

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