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Water → 3-Benzyl-1-(2-bromo-5-trifluoromethyl-benzyl)-1-ethyl-urea

HRID 554656
ノート
印刷プレビュー

反応式

HRID 554656 の反応式
[Br:1][C:2]1[CH:11]=[CH:10][C:9]([C:12]([F:15])([F:14])[F:13])=[CH:8][C:3]=1[CH2:4][NH:5][CH2:6][CH3:7].C(N(CC)CC)C.[CH2:23]([N:30]=[C:31]=[O:32])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.O>C(Cl)Cl>[CH2:23]([NH:30][C:31](=[O:32])[N:5]([CH2:4][C:3]1[CH:8]=[C:9]([C:12]([F:13])([F:14])[F:15])[CH:10]=[CH:11][C:2]=1[Br:1])[CH2:6][CH3:7])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 76639Benzyl isocyanateHCID 66603999(2-Bromo-5-trifluoromethyl-benzyl)-ethyl-amine

生成物 1

HCID 574588013-Benzyl-1-(2-bromo-5-trifluoromethyl-benzyl)-1-ethyl-urea

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To (2-bromo-5-trifluoromethyl-benzyl)-ethyl-amine (2.35 g, 8.33 mmol) in CH2Cl2 (24 mL) was added triethylamine (1.8 mL, 12.5 mmol), followed by benzyl isocyanate (1.22 mL, 10.0 mmol), and the reaction was stirred at room temperature for 50 minutes. The mixture was worked up with CH2Cl2 and H2O, and the combined organic layers were dried, filtered, and concentrated. The residue was dissolved in CH2Cl2 and filtered to remove solids, and the filtrate was purified by silica gel chromatography to give 3-benzyl-1-(2-bromo-5-trifluoromethyl-benzyl)-1-ethyl-urea.

後処理

  1. customthe combined organic layers were dried
  2. filtrationfiltered
  3. concentrationconcentrated
  4. dissolutionThe residue was dissolved in CH2Cl2
  5. filtrationfiltered
  6. customto remove solids
  7. customthe filtrate was purified by silica gel chromatography

出典と根拠

ORDレコード
ord-a2b1fcd13e0b4d7da9e2c55f092e963a
出典データセット
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08049015B2

反応ノート

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