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Benzene → HCID 19421674, 화합물

HRID 1613316
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HRID 1613316 반응식
P(Cl)(Cl)(Cl)=O.C1C=CC=CC=1.[CH3:12][O:13][C:14]1[CH:19]=[CH:18][C:17]([C:20]([C:29]2[CH:34]=[CH:33][C:32]([O:35][CH3:36])=[CH:31][CH:30]=2)(O)[CH:21]([CH3:27])[C:22]([O:24][CH2:25][CH3:26])=[O:23])=[CH:16][CH:15]=1>O>[CH3:36][O:35][C:32]1[CH:33]=[CH:34][C:29]([C:20]([C:17]2[CH:16]=[CH:15][C:14]([O:13][CH3:12])=[CH:19][CH:18]=2)=[C:21]([CH3:27])[C:22]([O:24][CH2:25][CH3:26])=[O:23])=[CH:30][CH:31]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 241BenzeneHCID 24813Phosphorus oxychlorideHCID 19421607Ethyl 3,3-bis(4-methoxyphenyl)-3-hydroxy-2-methylpropionate

생성물 1

HCID 19421674HCID 19421674, 화합물수율 90.8%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

4.10 ml of phosphorus oxychloride were dropped at from 5° to 10° C. onto 140 ml of a benzene solution containing 7.02 g of ethyl 3,3-bis(4-methoxyphenyl)-3-hydroxy- 2-methylpropionate (prepared as described in Preparation 106) on an ice bath. The reaction solution was then stirred for 3 hours at room temperature, after which it was poured into water and then extracted with diethyl ether three times. The combined ethereal extracts were washed with a saturated aqueous solution of sodium bicarbonate, with water and with a saturated aqueous solution of sodium chloride, after which it was dried over anhydrous sodium sulfate and condensed by evaporation under reduced pressure. The residue (6.72 g) was subjected to flash column chromatography through 100 g of silica gel. 6.04 g of the title compound were obtained as an oily substance from those fractions eluted with a 95:5 by volume mixture of hexane and ethyl acetate.

후처리

  1. extractionextracted with diethyl ether three times
  2. washThe combined ethereal extracts were washed with a saturated aqueous solution of sodium bicarbonate, with water and with a saturated aqueous solution of sodium chloride
  3. dry with materialafter which it was dried over anhydrous sodium sulfate and condensed by evaporation under reduced pressure

출처 및 근거

ORD 기록
ord-33330e728722487693ad2fb196701fef
출처 데이터셋
uspto-grants-1993_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05192766

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