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

HRID 65821

反応式

HRID 65821 の反応式
[C:1]([C:5]1[CH:20]=[CH:19][C:8]([CH2:9][CH2:10][O:11][C:12]2[CH:18]=[CH:17][C:15]([NH2:16])=[CH:14][CH:13]=2)=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].[CH3:21][O:22][N:23]([CH3:27])[C:24](Cl)=[O:25].N1C=CC=CC=1.[Cl-].[NH+]1C=CC=CC=1>O.C1(C)C=CC=CC=1>[C:1]([C:5]1[CH:20]=[CH:19][C:8]([CH2:9][CH2:10][O:11][C:12]2[CH:13]=[CH:14][C:15]([NH:16][C:24](=[O:25])[N:23]([O:22][CH3:21])[CH3:27])=[CH:17][CH:18]=2)=[CH:7][CH:6]=1)([CH3:4])([CH3:2])[CH3:3]

参加物

7

反応物 4

HCID 1049PyridineHCID 69401Einecs 211-027-4HCID 2734926N-methoxy-N-methylcarbamoyl chlorideHCID 227560014-(4-Tert-butylphenethyloxy)aniline

生成物 1

HCID 22756005N'-[4-(4-tert-butylphenethyloxy)phenyl]-N-methoxy-N-methylurea収率 26.1%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 1140Toluene溶媒

実験手順

A mixture of 26.9 g of 4-(4-tert-butylphenethyloxy)aniline, 13 g of N-methoxy-N-methylcarbamyl chloride, 10 ml of pyridine and 300 ml of toluene is heated under reflux for 7 hours. Thereafter, water is added to dissolve pyridinium chloride, and the separated toluene layer is washed with dilute hydrochloric acid, thoroughly washed with water and dried over anhydrous sodium sulfate. The solvent is then removed under reduced pressure, and the crude crystals obtained are repeatedly recrystallized from ethanol to obtain 9.3 g of N'-[4-(4-tert-butylphenethyloxy)phenyl]-N-methoxy-N-methylurea as white needles, M.P. 14°-15° C.

後処理

  1. temperatureis heated
  2. temperatureunder reflux for 7 hours
  3. washthe separated toluene layer is washed with dilute hydrochloric acid
  4. washthoroughly washed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe solvent is then removed under reduced pressure
  7. customthe crude crystals obtained
  8. customare repeatedly recrystallized from ethanol

出典と根拠

ORDレコード
ord-af08b02af2aa4bca8204bcf5fa2b9ff0
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…