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Pyridine → [6-(6-Isopentyloxyhexyloxy)-hexyl]-piperonyl ether

HRID 2398786
ノート
印刷プレビュー

反応式

HRID 2398786 の反応式
[CH2:1]([O:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][O:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][OH:20])[CH2:2][CH:3]([CH3:5])[CH3:4].[CH2:21](Br)[C:22]1[CH:30]=[CH:29][C:28]2[O:27][CH2:26][O:25][C:24]=2[CH:23]=1.C(=O)(O)[O-].[Na+].N1C=CC=CC=1>CCOCC>[CH2:1]([O:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][O:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][O:20][CH2:21][C:22]1[CH:30]=[CH:29][C:28]2[O:27][CH2:26][O:25][C:24]=2[CH:23]=1)[CH2:2][CH:3]([CH3:4])[CH3:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 1049PyridineHCID 516892Sodium BicarbonateHCID 64514231,3-Benzodioxole, 5-(bromomethyl)-HCID 214340396-(6-Isopentyloxyhexyloxy)-hexanol

生成物 1

HCID 68121476[6-(6-Isopentyloxyhexyloxy)-hexyl]-piperonyl ether

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

2.88 g (0.010 mol) of 6-(6-Isopentyloxyhexyloxy)-hexanol are mixed with 2.15 g (0.010 mol) of piperonyl bromide and 1.26 g (0.015 mol) of sodium bicarbonate and the mixture is stirred at 80° for 18 hours and then at 120° C. for 6 hours. 1.0 cc of pyridine is added to the reaction mixture which is heated to 80° over the course of 2 hours. The reaction mixture is cooled, taken up in ether, washed with 2N sulphuric acid, water and saturated sodium chloride solution, dried over magnesium sulphate and evaporated. After chromatography of the residue on silica gel with hexane/acetone (98:2) and (96:4), [6-(6-Isopentyloxyhexyloxy)-hexyl]-piperonyl ether is obtained as a colourless oil.

後処理

  1. waitat 120° C. for 6 hours
  2. temperatureis heated to 80° over the course of 2 hours
  3. temperatureThe reaction mixture is cooled
  4. washwashed with 2N sulphuric acid, water and saturated sodium chloride solution
  5. dry with materialdried over magnesium sulphate
  6. customevaporated

出典と根拠

ORDレコード
ord-c5eced5aaf984491a2b68f6633d0e405
出典データセット
uspto-grants-1977_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04025641

反応ノート

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