Sodium Iodide → HCID 10894686、化合物

HRID 1289398ノート

反応式

HRID 1289398 の反応式
Br[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][O:14][CH2:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.[I-:22].[Na+]>CC(C)=O>[I:22][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][O:14][CH2:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1

参加物

4

反応物 2

HCID 5238Sodium IodideHCID 11100339Benzene, [[(12-bromododecyl)oxy]methyl]-

生成物 1

HCID 10894686HCID 10894686、化合物収率 104.7%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

First, 12.4 g of 1-bromo-12-benzyloxydodecane, 6.3 g of sodium iodide, and 125 ml of acetone were placed in a 200 ml flask whose content was replaced with argon. Then, the mixture was stirred under reflux for 5 hours. An insoluble matter was filtered away and a filtrate was concentrated. Thereafter, ether was introduced into the residue. The ether layer was washed with water and dried over anhydrous sodium sulfate. Thereafter, the solvent was distilled away. The residue was purified by silica gel column chromatography (eluent: toluene/hexane=1/1) to obtain 14.7 g of 1-iodo-12-benzyloxydodecane (Y: 100%). The compound thus obtained had a purity of 96.1% by GC.

後処理

  1. temperatureunder reflux for 5 hours
  2. filtrationAn insoluble matter was filtered away
  3. concentrationa filtrate was concentrated
  4. additionThereafter, ether was introduced into the residue
  5. washThe ether layer was washed with water
  6. dry with materialdried over anhydrous sodium sulfate
  7. distillationThereafter, the solvent was distilled away
  8. customThe residue was purified by silica gel column chromatography (eluent: toluene/hexane=1/1)

出典と根拠

ORDレコード
ord-2d31262407d24d73bd6ec31c13ba9723
出典データセット
uspto-grants-1998_05
特許番号
US05750213

反応ノート

読み込み中…