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

HRID 250819

反応式

HRID 250819 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, 1.5 eq) of heptyl isocyanate are added to a solution of 2.5 g (13 mmol, 1 eq) of (3-bromophenyl)methylamine in 10 ml of tetrahydrofuran in the presence of 2 ml of triethylamine. The reaction mixture is stirred for 12 hours at r.t. The reaction is stopped by addition of 2 mL of water and then extracted with ethyl acetate. The organic phases are combined and dried over sodium sulfate. The solvents are evaporated off and the residue is then chromatographed on silica gel (70/30 heptane/ethyl acetate). 3.4 g of 1-(3-bromophenyl)-3-heptyl-1-methylurea in solid form are obtained. Yield=77%

後処理

  1. extractionextracted with ethyl acetate
  2. dry with materialdried over sodium sulfate
  3. customThe solvents are evaporated off
  4. customthe residue is then chromatographed on silica gel (70/30 heptane/ethyl acetate)

出典と根拠

ORDレコード
ord-7bce2084f23d4fab908e6bf2226b1626
出典データセット
uspto-grants-2011_01
特許番号
US07863332B2

関連ノート

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