Triethylamine → Monoisouron

HRID 1763189노트

반응식

HRID 1763189 반응식
[NH2:1][C:2]1[CH:6]=[C:5]([C:7]([CH3:10])([CH3:9])[CH3:8])[O:4][N:3]=1.[CH3:11][N:12]=[C:13]=[O:14].C(N(CC)CC)C>C1C=CC=CC=1>[CH3:11][NH:12][C:13]([NH:1][C:2]1[CH:6]=[C:5]([C:7]([CH3:10])([CH3:9])[CH3:8])[O:4][N:3]=1)=[O:14]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 12228Methyl IsocyanateHCID 1714733-Isoxazolamine, 5-(1,1-dimethylethyl)-

생성물 1

HCID 186687Monoisouron수율 91.3%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

To a solution of 3-amino-5-t-butylisoxazole (16.82 g) in anhydrous benzene (140 ml), methyl isocyanate (8.90 g) and triethylamine (0.5 ml) are added. The resulting mixture is stirred at room temperature for about 8 hours, allowed to stand overnight and refluxed for 1 hour. After ice cooling, the reaction mixture is filtered to give a precipitate, which is recrystallized from ethyl acetate to give 1-methyl-3-(5-t-butyl-3-isoxazolyl)urea (21.61 g) as colorless needles melting at 187.0° to 187.5° C.

후처리

  1. waitto stand overnight
  2. temperaturerefluxed for 1 hour
  3. filtrationAfter ice cooling, the reaction mixture is filtered
  4. customto give a precipitate, which
  5. customis recrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-a9426200a02b4ac78ad9eba5e3a3e641
출처 데이터셋
uspto-grants-1978_09
특허 번호
US04111680

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