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

HRID 1289408ノート

反応式

HRID 1289408 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-d5eb4f851bc844469578de3f58a3888c
出典データセット
uspto-grants-1998_05
特許番号
US05750213

反応ノート

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