Water → 1-(3-Bromophenyl)-3-heptyl-1-methylurea

HRID 1808300

반응식

HRID 1808300 반응식
[CH2:1]([N:8]=[C:9]=[O:10])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH3:7].[Br:11][C:12]1[CH:13]=[C:14](CN)[CH:15]=[CH:16][CH:17]=1.[CH2:20]([N:22](CC)CC)C.O>O1CCCC1>[Br:11][C:12]1[CH:13]=[C:14]([N:22]([CH3:20])[C:9]([NH:8][CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH3:7])=[O:10])[CH:15]=[CH:16][CH:17]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 138341n-Heptyl isocyanateHCID 457587Benzenemethanamine, 3-bromo-

생성물 1

HCID 116168371-(3-Bromophenyl)-3-heptyl-1-methylurea수율 77%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

3.2 ml (20 mmol) of heptyl isocyanate are added to a solution of 2.5 g (13 mmol) of (3-bromophenyl)methyl-amine, thus prepared, in 10 ml of tetrahydrofuran in the presence of 2 ml of triethylamine. The reaction mixture is stirred at ambient temperature for 12 hours. The reaction is halted by the addition of 2 ml of water and then extracted with ethyl acetate. The organic phases are combined and dried over sodium sulphate. The solvents are evaporated and then the residue is purified by chromatography on a column of silica eluted with a heptane/ethyl acetate 70/30 mixture. 3.4 g (77%) of 1-(3-bromophenyl)-3-heptyl-1-methylurea are obtained in the solid form.

후처리

  1. extractionextracted with ethyl acetate
  2. dry with materialdried over sodium sulphate
  3. customThe solvents are evaporated
  4. customthe residue is purified by chromatography on a column of silica
  5. washeluted with a heptane/ethyl acetate 70/30 mixture

출처 및 근거

ORD 기록
ord-c5061c1d69ba4062942aad5a37dbd001
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08357819B2

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