Sodium Iodide → 2,2-Bis(6-benzyloxyhexyl)ethyl iodide

HRID 1289408노트

반응식

HRID 1289408 반응식
[CH2:1]([O:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH:15]([CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][O:24][CH2:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)[CH2:16]Br)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[I-:32].[Na+].CC(=O)CC>O>[CH2:1]([O:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH:15]([CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][O:24][CH2:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)[CH2:16][I:32])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 5238Sodium IodideHCID 6569Methyl Ethyl KetoneHCID 189208332,2-Bis(6-benzyloxyhexyl)ethyl bromide

생성물 1

HCID 189208712,2-Bis(6-benzyloxyhexyl)ethyl iodide수율 91.2%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

First, 6 g of 2,2-bis(6-benzyloxyhexyl)ethyl bromide, 2.19 g of sodium iodide, and 150 ml of 2-butanone were placed in a 300 ml flask. The mixture was stirred under reflux for 16 hours. The reaction mixture was poured into water, and an organic layer was extracted with ether. The ether layer was washed with water and dried over anhydrous sodium sulfate. The solvent was distilled away. The residue was purified by silica gel column chromatography (eluent: toluene) to obtain 6 g of 2,2-bis(6-benzyloxyhexyl)ethyl iodide (Y: 91.2%). The compound thus obtained had a purity of 95.3% by HPLC.

후처리

  1. temperatureunder reflux for 16 hours
  2. extractionan organic layer was extracted with ether
  3. washThe ether layer was washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationThe solvent was distilled away
  6. customThe residue was purified by silica gel column chromatography (eluent: toluene)

출처 및 근거

ORD 기록
ord-d5eb4f851bc844469578de3f58a3888c
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05750213

반응 노트

불러오는 중…