Water → N,N-Diethyl-N'-phenylurea

HRID 965541ノート

反応式

HRID 965541 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:8]([N:10]([CH2:14][CH3:15])[C:11](Cl)=[O:12])[CH3:9].O>N1C=CC=CC=1>[CH2:8]([N:10]([CH2:14][CH3:15])[C:11](=[O:12])[NH:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[CH3:9]

参加物

5

反応物 3

HCID 962WaterHCID 6115AnilineHCID 6916Diethylcarbamoyl chloride

生成物 1

HCID 13906N,N-Diethyl-N'-phenylurea収率 63%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒2 回

実験手順

A solution of 10 g of aniline in 50 ml of pyridine is cooled to 0° C. and a solution of 14.56 g of diethylcarbamoyl chloride in 10 ml of pyridine is added slowly. The mixture is stirred for 6 hours, the temperature being allowed to rise to RT, and is then poured into water. It is extracted with AcOEt, washed with water and with a 5% solution of potassium hydrogensulfate, dried over sodium sulfate and evaporated under vacuum. The residue is chromatographed on silica using DCM and then a DCM/AcOEt mixture (90/10; v/v) as the eluent to give 13 g of the expected product, which is used as such in the next step.

後処理

  1. customto rise to RT
  2. extractionIt is extracted with AcOEt
  3. washwashed with water and with a 5% solution of potassium hydrogensulfate
  4. dry with materialdried over sodium sulfate
  5. customevaporated under vacuum
  6. customThe residue is chromatographed on silica

出典と根拠

ORDレコード
ord-9f1c1b3f15714db7a8f5655ef923b364
出典データセット
uspto-grants-1998_06
特許番号
US05773612

反応ノート

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