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Methyl iodide → HCID 178444452, 화합물

HRID 2226075
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HRID 2226075 반응식
[CH2:1]([C@H:6]1[CH2:11][CH2:10][C@H:9]([CH2:12][CH2:13][CH2:14][CH2:15][C:16]2[CH:21]=[CH:20][C:19]([OH:22])=[CH:18][CH:17]=2)[CH2:8][CH2:7]1)[CH2:2][CH2:3][CH2:4][CH3:5].CI.[C:25](=O)([O-])[O-].[K+].[K+].CC(=O)CC>O>[CH3:25][O:22][C:19]1[CH:18]=[CH:17][C:16]([CH2:15][CH2:14][CH2:13][CH2:12][C@H:9]2[CH2:8][CH2:7][C@H:6]([CH2:1][CH2:2][CH2:3][CH2:4][CH3:5])[CH2:11][CH2:10]2)=[CH:21][CH:20]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6328Methyl iodideHCID 6569Methyl Ethyl KetoneHCID 11430Potassium CarbonateHCID 178444450HCID 178444450, 화합물

생성물 1

HCID 178444452HCID 178444452, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 0.3 g of 4-[4-(trans-4-pentylcyclohexyl)-1-butyl]phenol, 0.14 g of methyl iodide, 0.6 g of potassium carbonate and 50 ml of absolute butanone was heated to reflux overnight. Subsequently, the cooled reaction mixture was poured into water and extracted three times with 50 ml of diethyl ether each time. The combined organic phases were washed with 500 ml of water, dried over magnesium sulfate, filtered and concentrated. Chromatography of the residue on silica gel with toluene and recrystallization from ethanol gave pure 1-methoxy-4-[4-(trans-4-pentylcyclohexyl)-1-butyl]benzene with m.p. (C-I) 27° C. and cl.p. (SB -I) 16° C.

후처리

  1. temperaturewas heated
  2. temperatureto reflux overnight
  3. customSubsequently, the cooled reaction mixture
  4. extractionextracted three times with 50 ml of diethyl ether each time
  5. washThe combined organic phases were washed with 500 ml of water
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customChromatography of the residue on silica gel with toluene and recrystallization from ethanol

출처 및 근거

ORD 기록
ord-4cde085360454d219fcf32adb317f2aa
출처 데이터셋
uspto-grants-1994_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05346647

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