1-Bromodecane → 1-Decyl-2-methyl-1H-imidazole

HRID 53467

反応式

HRID 53467 の反応式
[CH3:1][C:2]1[NH:3][CH:4]=[CH:5][N:6]=1.Br[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17].[OH-].[Na+]>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.C1(C)C=CC=CC=1>[CH2:8]([N:3]1[CH:4]=[CH:5][N:6]=[C:2]1[CH3:1])[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17]

参加物

6

反応条件

温度
65 °C

実験手順

A mixture of 2-methylimidazole (12.3 g; 0.15 mol), 1-bromodecane (33.15 g; 0.15 mol), sodium hydroxide solution (69.5 ml. of 11.5M solution; 0.8 mol) and tetra-n-butylammonium bromide (1.95 g; 0.006 mol) in toluene (300 ml) was stirred rapidly for 3 hours at 65° C. After cooling to between 20° and 25° C., the toluene layer was separated and extracted with 5M HCl solution (150 ml). The extract neutralised with sodium bicarbonate and extracted many times into hexane. The hexane solution was dried over magnesium sulphate and evaporated to dryness to give an oil (25 g; 75% theory).

後処理

  1. temperatureAfter cooling to between 20° and 25° C.
  2. customthe toluene layer was separated
  3. extractionextracted with 5M HCl solution (150 ml)
  4. extractionThe extract neutralised with sodium bicarbonate and extracted many times into hexane
  5. dry with materialThe hexane solution was dried over magnesium sulphate
  6. customevaporated to dryness
  7. customto give an oil (25 g; 75% theory)

出典と根拠

ORDレコード
ord-c257b3c794de4fd7976632967b32723a
出典データセット
uspto-grants-1997_04
特許番号
US05620595

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