Sodium Iodide → HCID 10894686, 화합물

HRID 1289398노트

반응식

HRID 1289398 반응식
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

참가 물질

4

반응물 2

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

생성물 1

HCID 10894686HCID 10894686, 화합물수율 104.7%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-2d31262407d24d73bd6ec31c13ba9723
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05750213

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