Pyridine → N'-[4-(4-isopropylphenethyloxy)phenyl]-N-methoxy-N-methylurea

HRID 65820

反応式

HRID 65820 の反応式
[CH:1]([C:4]1[CH:22]=[CH:21][C:7]([CH2:8][CH2:9][O:10][C:11]2[CH:16]=[CH:15][C:14]([NH:17][C:18](Cl)=[O:19])=[CH:13][CH:12]=2)=[CH:6][CH:5]=1)([CH3:3])[CH3:2].N1C=CC=CC=1.[CH3:29][NH:30][O:31][CH3:32]>C1(C)C=CC=CC=1>[CH:1]([C:4]1[CH:22]=[CH:21][C:7]([CH2:8][CH2:9][O:10][C:11]2[CH:16]=[CH:15][C:14]([NH:17][C:18](=[O:19])[N:30]([O:31][CH3:32])[CH3:29])=[CH:13][CH:12]=2)=[CH:6][CH:5]=1)([CH3:3])[CH3:2]

参加物

5

反応物 3

HCID 1049PyridineHCID 14232N,O-DimethylhydroxylamineHCID 227559994-(4-Isopropylphenethyloxy)phenylcarbamyl chloride

生成物 1

HCID 22756003N'-[4-(4-isopropylphenethyloxy)phenyl]-N-methoxy-N-methylurea収率 42%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

Into a solution of 10.6 g of 4-(4-isopropylphenethyloxy)phenylcarbamyl chloride in 200 ml of toluene are added 4 ml of pyridine and a solution of 2.5 g of N,O-dimethylhydroxylamine in 50 ml of toluene at a temperature below 20° C. The mixture is heated under reflux for 4 hours. The reaction mixture is then poured into ice water, and the separated organic layer is washed with dilute hydrochloric acid, thoroughly washed with water and dried over anhydrous sodium sulfate. The solvent is removed under reduced pressure, and the crude crystals are recrystallized from ethanol to obtain 4.8 g of N'-[4-(4-isopropylphenethyloxy)phenyl]-N-methoxy-N-methylurea as white needles, M.P. 81°-82° C.

後処理

  1. customat a temperature below 20° C
  2. temperatureThe mixture is heated
  3. temperatureunder reflux for 4 hours
  4. washthe separated organic layer is washed with dilute hydrochloric acid
  5. washthoroughly washed with water
  6. dry with materialdried over anhydrous sodium sulfate
  7. customThe solvent is removed under reduced pressure
  8. customthe crude crystals are recrystallized from ethanol

出典と根拠

ORDレコード
ord-ab87deb8c12c442892eeaba8a286c718
出典データセット
uspto-grants-1978_12
特許番号
US04129436

関連ノート

読み込み中…