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Water → HCID 178444453、化合物

HRID 2226074
ノート
印刷プレビュー

反応式

HRID 2226074 の反応式
[Br-].[CH2:2]([O:6][C:7]1[CH:12]=[CH:11][C:10]([CH2:13][P+](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=[CH:9][CH:8]=1)[CH2:3][CH2:4][CH3:5].[CH2:33]([C@H:38]1[CH2:43][CH2:42][C@H:41]([CH2:44][CH2:45][CH:46]=O)[CH2:40][CH2:39]1)[CH2:34][CH2:35][CH2:36][CH3:37].O>COC(C)(C)C>[CH2:2]([O:6][C:7]1[CH:8]=[CH:9][C:10]([CH:13]=[CH:46][CH2:45][CH2:44][C@H:41]2[CH2:40][CH2:39][C@H:38]([CH2:33][CH2:34][CH2:35][CH2:36][CH3:37])[CH2:43][CH2:42]2)=[CH:11][CH:12]=1)[CH2:3][CH2:4][CH3:5]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 21917838(4-Butoxybenzyl)triphenylphosphonium bromideHCID 178444474HCID 178444474、化合物

生成物 1

HCID 178444453HCID 178444453、化合物収率 82.6%

試薬・触媒・溶媒 1

HCID 15413tert-Butyl methyl ether溶媒2 回

反応条件

温度
0 °C

実験手順

A mixture of 54 g of (4-butyloxyphenyl)methyl-triphenylphosphonium bromide and 450 ml of absolute t-butyl methyl ether was treated with 12 g of solid potassium t-butylate at 0° C. and while gassing with nitrogen. After completion of the addition the reaction mixture was stirred at 0° C. for a further 15 minutes (whereby a deep orange coloration resulted) and then treated within 30 minutes at 0° C. with a solution of 15 g of 3-(trans-4-pentylcyclohexyl)propionaldehyde in 150 ml of absolute t-butyl methyl ether. Subsequently, the reaction mixture was stirred at room temperature overnight and then poured into 1000 ml of water and extracted three times with 200 ml of diethyl ether each time. The organic phases were washed twice with 500 ml of concentrated sodium chloride solution each time, dried over magnesium sulfate, filtered and subsequently concentrated. Chromatography of the residue on silica gel with hexane/toluene (vol. 4:1) gave 21 g of 1-butyloxy-4-[4-(trans-4 -pentylcyclohexyl)-1-butenyl]benzene (cis/trans mixture). Recrystallization from ethanol gave pure trans isomer with m.p. (C-SB) 46° C., SB --SA 74° C., SA --N 76° C. and cl.p. (N--I) 91° C.

後処理

  1. additionAfter completion of the addition the reaction mixture
  2. customresulted) and
  3. stirringSubsequently, the reaction mixture was stirred at room temperature overnight
  4. extractionextracted three times with 200 ml of diethyl ether each time
  5. washThe organic phases were washed twice with 500 ml of concentrated sodium chloride solution each time
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationsubsequently concentrated

出典と根拠

ORDレコード
ord-9596eb0180bf42f5b94e1d38c03af358
出典データセット
uspto-grants-1994_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05346647

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート