Toluene → 3-(3-Fluoro-4-isopropyl-phenyl)-5-methyltetrahydro-1,3,5-oxadiazin-4-one

HRID 262931

반응식

HRID 262931 반응식
[F:1][C:2]1[CH:3]=[C:4]([NH:11][C:12]([NH:14][CH3:15])=[O:13])[CH:5]=[CH:6][C:7]=1[CH:8]([CH3:10])[CH3:9].CN(C)[CH:18]=[O:19].[C:21]1(C)C=CC=CC=1>C1(C)C=CC(S(O)(=O)=O)=CC=1>[F:1][C:2]1[CH:3]=[C:4]([N:11]2[C:12](=[O:13])[N:14]([CH3:21])[CH2:15][O:19][CH2:18]2)[CH:5]=[CH:6][C:7]=1[CH:8]([CH3:9])[CH3:10]

참가 물질

6

반응물 4

HCID 1140TolueneHCID 6228DimethylformamideHCID 21317057N-(3-Fluoro-4-isopropyl-phenyl)-N'-methyl-ureaHCID 178486302HCID 178486302, 화합물

생성물 1

HCID 213170583-(3-Fluoro-4-isopropyl-phenyl)-5-methyltetrahydro-1,3,5-oxadiazin-4-one수율 82%

시약·촉매·용매 1

HCID 6101p-Toluenesulfonic acid촉매

반응 조건

온도
80 °C

실험 절차

N-(3-Fluoro-4-isopropyl-phenyl)-N'-methyl-urea (one mol=210 g.) and polyoxymethylene (1 mol=90 g.) are dissolved in toluene (800 cc.) in the presence of para-toluenesulphonic acid (0.3 mol=51.6 g.) as a catalyst and of dimethylformamide (0.3 mol=22 g.), and the mixture is heated for 15 minutes at 80° C. After having washed the solution with water and then concentrated it, 3-(3-fluoro-4-isopropyl-phenyl)-5-methyltetrahydro-1,3,5-oxadiazin-4-one is obtained in the form of an oil which is purified by dissolving in hot hexane and recrystallising.

후처리

  1. washAfter having washed the solution with water
  2. concentrationconcentrated it

출처 및 근거

ORD 기록
ord-510a4bf1a90642f583f7a61a6c0b2b29
출처 데이터셋
uspto-grants-1979_05
특허 번호
US04155747

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