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Potassium Carbonate → 1-[p-(N',N'-dimethylureido)-phenoxy]-2-hydroxy-3-isopropylaminopropane

HRID 1112236
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HRID 1112236 반응식
[CH3:1][N:2]([CH3:13])[C:3](=[O:12])[NH:4][C:5]1[CH:10]=[CH:9][C:8]([OH:11])=[CH:7][CH:6]=1.[CH:14]([NH:17][CH2:18][CH:19]([OH:22])[CH2:20]Cl)([CH3:16])[CH3:15].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[CH3:1][N:2]([CH3:13])[C:3](=[O:12])[NH:4][C:5]1[CH:10]=[CH:9][C:8]([O:11][CH2:20][CH:19]([OH:22])[CH2:18][NH:17][CH:14]([CH3:16])[CH3:15])=[CH:7][CH:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 3014146Urea, N'-(4-hydroxyphenyl)-N,N-dimethyl-HCID 126246123-Isopropylamino-2-hydroxy-1-chloropropane

생성물 1

HCID 126663201-[p-(N',N'-dimethylureido)-phenoxy]-2-hydroxy-3-isopropylaminopropane

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mixture of 20 g of p-(N',N'-dimethylureido)-phenol, 15 g of 3-isopropylamino-2-hydroxy-1-chloropropane, and 20 g of finely ground potassium carbonate in 250 ml of acetone is stirred at 50° for 5 hours. The solid part of the mixture is filtered off and the acetone solution is evaporated in a vacuum. The residue is dissolved in 100 ml of 2N hydrochloric acid, the undissolved part is filtered off and the remaining mixture is extracted with methylene chloride. The aqueous phase is rendered alkaline by adding 2N sodium hydroxide solution and is extracted with methylene chloride. After the evaporation of the solvent, 1-[p-(N',N'-dimethylureido)-phenoxy]-2-hydroxy-3-isopropylaminopropane is isolated which melts at 138°-139° after recrystallisation from benzene and has the formula ##STR22##

후처리

  1. filtrationThe solid part of the mixture is filtered off
  2. customthe acetone solution is evaporated in a vacuum
  3. dissolutionThe residue is dissolved in 100 ml of 2N hydrochloric acid
  4. filtrationthe undissolved part is filtered off
  5. extractionthe remaining mixture is extracted with methylene chloride
  6. additionby adding 2N sodium hydroxide solution
  7. extractionis extracted with methylene chloride
  8. customAfter the evaporation of the solvent

출처 및 근거

ORD 기록
ord-2976261cc0ad4359bcb1af5340f0752e
출처 데이터셋
uspto-grants-1978_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04120978

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