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

HRID 65821

반응식

HRID 65821 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 1140Toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-af08b02af2aa4bca8204bcf5fa2b9ff0
출처 데이터셋
uspto-grants-1978_12
특허 번호
US04129436

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