Triethylamine → HCID 67272794, 화합물

HRID 250908노트

반응식

HRID 250908 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 67272794HCID 67272794, 화합물수율 287.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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%

후처리

  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

출처 및 근거

ORD 기록
ord-62e8a140f8a64c8d927b6b9af5bc088b
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07863332B2

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