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

HRID 1808300

反応式

HRID 1808300 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 116168371-(3-Bromophenyl)-3-heptyl-1-methylurea収率 77%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c5061c1d69ba4062942aad5a37dbd001
出典データセット
uspto-grants-2013_01
特許番号
US08357819B2

関連ノート

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