Hydrochloric Acid → 1,5-Bis(4-methoxyphenyl)pentane

HRID 979063노트

반응식

HRID 979063 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][CH2:10][C:11](=O)[CH2:12][CH2:13][C:14]2[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=2)=[CH:5][CH:4]=1.O1CCOCC1.Cl>[Zn].O>[CH3:21][O:20][C:17]1[CH:16]=[CH:15][C:14]([CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][C:6]2[CH:5]=[CH:4][C:3]([O:2][CH3:1])=[CH:8][CH:7]=2)=[CH:19][CH:18]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric Acid2회HCID 312751,4-DioxaneHCID 2801509HCID 2801509, 화합물

생성물 1

HCID 132200991,5-Bis(4-methoxyphenyl)pentane수율 111%

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 962Water용매

실험 절차

A mixture of 1,5-bis(4-methoxyphenyl)pentan-3-one of Example 7 (57 g, 0.19 mole), amalgamated zinc (200 g), dioxane (250 ml), concentrated hydrochloric acid (250 ml) and 150 ml of water was refluxed overnight. A further 50 ml of concentrated hydrochloric acid was added after the first 6 hours. The organic layer was separated, diluted with ether, washed with water, dried over anhydrous magnesium sulfate and concentrated to give 60 g of a thick oil. NMR and mass spectra confirmed the structure.

후처리

  1. temperaturewas refluxed overnight
  2. customThe organic layer was separated
  3. additiondiluted with ether
  4. washwashed with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-664cca7836f34f31996087dc05955dff
출처 데이터셋
uspto-grants-1987_05
특허 번호
US04666909

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