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Triethylamine → 2-{4-(3-Ethoxy-2-hydroxypropoxy)phenylcarbamoyl}ethyl methyl sulfide

HRID 637532
ノート
印刷プレビュー

反応式

HRID 637532 の反応式
C(N(CC)CC)C.[CH2:8]([O:10][CH2:11][CH:12]([OH:22])[CH2:13][O:14][C:15]1[CH:21]=[CH:20][C:18]([NH2:19])=[CH:17][CH:16]=1)[CH3:9].[CH3:23][S:24][CH2:25][CH2:26][C:27](Cl)=[O:28]>CN(C)C=O>[CH3:23][S:24][CH2:25][CH2:26][C:27](=[O:28])[NH:19][C:18]1[CH:17]=[CH:16][C:15]([O:14][CH2:13][CH:12]([OH:22])[CH2:11][O:10][CH2:8][CH3:9])=[CH:21][CH:20]=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 8471TriethylamineHCID 107748571-(4-Aminophenoxy)-3-ethoxypropan-2-olHCID 129214403-(Methylthio)propionyl Chloride

生成物 1

HCID 105912962-{4-(3-Ethoxy-2-hydroxypropoxy)phenylcarbamoyl}ethyl methyl sulfide

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Dissolved in 4 ml of dimethylformamide were 1.46 g of triethylamine and 1.52 g of 4-(3-ethoxy-2-hydroxypropoxy)aniline. A 1.10 g quantity of 3-methylmercaptopropionyl chloride was added to the solution with ice-cooling. The mixture was stirred at room temperature for 12 hours and the reaction mixture was concentrated. The residue was extracted with chloroform and the chloroform layer was washed successively with 1N hydrochloric acid, a saturated aqueous solution of sodium hydrogencarbonate and water and concentrated. Ether was added to the residue and the crystals formed were filtered off to give 1.52 g of 2-{4-(3-ethoxy-2-hydroxypropoxy)phenylcarbamoyl}ethyl methyl sulfide in 67.4%, M.P. 79° to 81° C.

後処理

  1. temperaturecooling
  2. concentrationthe reaction mixture was concentrated
  3. extractionThe residue was extracted with chloroform
  4. washthe chloroform layer was washed successively with 1N hydrochloric acid
  5. concentrationa saturated aqueous solution of sodium hydrogencarbonate and water and concentrated
  6. additionEther was added to the residue
  7. customthe crystals formed
  8. filtrationwere filtered off

出典と根拠

ORDレコード
ord-f8d0eb0abaaa49c7844a183232104acf
出典データセット
uspto-grants-1985_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04556737

反応ノート

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