Triethylamine → HCID 67272794、化合物

HRID 250908ノート

反応式

HRID 250908 の反応式
[CH2:1]([N:6]=[C:7]=[O:8])[CH2:2][CH2:3][CH2:4][CH3:5].[Br:9][C:10]1[CH:11]=[C:12](CN)[CH:13]=[CH:14][CH:15]=1.[CH2:18]([N:20](CC)CC)C>ClCCl>[Br:9][C:10]1[CH:11]=[C:12]([N:20]([CH3:18])[C:7]([NH:6][CH2:1][CH2:2][CH2:3][CH2:4][CH3:5])=[O:8])[CH:13]=[CH:14][CH:15]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 206036Pentane, 1-isocyanato-HCID 457587Benzenemethanamine, 3-bromo-

生成物 1

HCID 67272794HCID 67272794、化合物収率 287.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of 50.0 g (0.442 mol, 1 eq) of pentyl isocyanate in 50 mL of dichloromethane is added to a mixture of 82.2 g (0.442 mol, 1 eq) of (3-bromophenyl)methylamine in 250 mL of dichloromethane in the presence of 20 mL (0.143 mol, 0.3 eq) of triethylamine. The reaction medium is refluxed for 3 days and then hydrolyzed in 200 mL of 1N hydrochloric acid solution and extracted with ethyl acetate. The organic phases are combined, washed with water and sodium chloride, and evaporated. 123 g of 1-(3-bromophenyl)-1-methyl-3-pentylurea are obtained. Yield=93%

後処理

  1. temperatureThe reaction medium is refluxed for 3 days
  2. extractionhydrolyzed in 200 mL of 1N hydrochloric acid solution and extracted with ethyl acetate
  3. washwashed with water and sodium chloride
  4. customevaporated

出典と根拠

ORDレコード
ord-62e8a140f8a64c8d927b6b9af5bc088b
出典データセット
uspto-grants-2011_01
特許番号
US07863332B2

反応ノート

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