3-(Trifluoromethyl)aniline → N,N'-Di-(m-trifluoromethylphenyl)urea

HRID 1243646노트

반응식

HRID 1243646 반응식
[F:1][C:2]([F:13])([F:12])[C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([N:9]=[C:10]=[O:11])[CH:4]=1.[F:14][C:15]([F:24])([F:23])[C:16]1[CH:17]=[C:18]([CH:20]=[CH:21][CH:22]=1)[NH2:19]>ClCCl>[F:1][C:2]([F:12])([F:13])[C:3]1[CH:4]=[C:5]([NH:9][C:10]([NH:19][C:18]2[CH:20]=[CH:21][CH:22]=[C:16]([C:15]([F:14])([F:23])[F:24])[CH:17]=2)=[O:11])[CH:6]=[CH:7][CH:8]=1

참가 물질

4

반응물 2

HCID 73753-(Trifluoromethyl)anilineHCID 94833-(Trifluoromethyl)phenyl isocyanate

생성물 1

HCID 136250N,N'-Di-(m-trifluoromethylphenyl)urea수율 97%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

In a round bottom flask under nitrogen, α,α,α-trifluro-m-tolyl isocyanate (3 g, 16 mmol) was dissolved in anhydrous dichloromethane (40 mL). 3-(Trifluoromethyl) aniline (2 g, 12.4 mmol) was added through a syringe at room temperature. A precipitate was formed 15 minutes after the completion of the addition. The reaction was left to stir overnight at room temperature. The next day the white solid was collected by filtration, washed with dichloromethane and dried. This solid corresponds to the desired urea. (4.2 g, 97% yield). 1H NMR (400 MHz, DMSO) δ 7.35 (d, 2H), 7.55 (m, 2 H), 7.6 (d, 2H), 8.05 (s, 2H). MS calculated=m/e 348, found=m/e 348.

후처리

  1. customA precipitate was formed 15 minutes
  2. additionafter the completion of the addition
  3. waitThe reaction was left
  4. filtrationThe next day the white solid was collected by filtration
  5. washwashed with dichloromethane
  6. customdried

출처 및 근거

ORD 기록
ord-06aa03ec397f43fa9e11421b67188a10
출처 데이터셋
uspto-grants-2006_10
특허 번호
US07119120B2

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