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

HRID 1243646ノート

反応式

HRID 1243646 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-06aa03ec397f43fa9e11421b67188a10
出典データセット
uspto-grants-2006_10
特許番号
US07119120B2

反応ノート

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