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Water → HCID 178444453, 화합물

HRID 2226074
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HRID 2226074 반응식
[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]
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5

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HCID 962WaterHCID 21917838(4-Butoxybenzyl)triphenylphosphonium bromideHCID 178444474HCID 178444474, 화합물

생성물 1

HCID 178444453HCID 178444453, 화합물수율 82.6%

시약·촉매·용매 1

HCID 15413tert-Butyl methyl ether용매2회

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온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9596eb0180bf42f5b94e1d38c03af358
출처 데이터셋
uspto-grants-1994_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05346647

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