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

HRID 1581069
ノート
印刷プレビュー

反応式

HRID 1581069 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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 ##SPC6##

後処理

  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

出典と根拠

ORDレコード
ord-163c6c30691d48c2a5e9791940fc7bb3
出典データセット
uspto-grants-1976_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03935259

反応ノート

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