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

HRID 728825노트

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HRID 728825 반응식
[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

참가 물질

7

반응물 3

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

생성물 1

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

시약·촉매·용매 3

HCID 887Methanol용매HCID 14797Potassium Hydroxide용매HCID 178502851MeOHis용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5c31cd1d8aa349ea9f35a71853cf0cf4
출처 데이터셋
uspto-grants-1991_09
특허 번호
US05051423

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