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Calcium Carbonate → Benzaldehyde, 3-(4-fluorophenoxy)-

HRID 704816
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반응식

HRID 704816 반응식
Br[CH:2](Br)[C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([O:9][C:10]2[CH:15]=[CH:14][C:13]([F:16])=[CH:12][CH:11]=2)[CH:4]=1.C(=O)([O-])[O-:19].[Ca+2]>C(O)C.O>[F:16][C:13]1[CH:14]=[CH:15][C:10]([O:9][C:5]2[CH:4]=[C:3]([CH:8]=[CH:7][CH:6]=2)[CH:2]=[O:19])=[CH:11][CH:12]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 10112Calcium CarbonateHCID 20073369HCID 20073369, 화합물

생성물 1

HCID 3085320Benzaldehyde, 3-(4-fluorophenoxy)-수율 92.4%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

A solution of the product of step (b) (16.04 g) in a mixture of ethanol (100 ml) and water (25 ml) was treated with precipitated calcium carbonate (13.37 g) and the mixture refluxed for 20 hours. After cooling, the mixture was filtered, the filtrate stripped, and the residue taken up in 2 M aqu. HCl (100 ml) and extracted with ether (200 ml). The extract was washed with water (100 ml), dried over Na2SO4 and stripped to give a pale yellow oil which was distilled under reduced pressure to give the desired product (8.90 g), bp 100°-130° C./0.2 mm Hg.

후처리

  1. temperaturethe mixture refluxed for 20 hours
  2. temperatureAfter cooling
  3. filtrationthe mixture was filtered
  4. extractionHCl (100 ml) and extracted with ether (200 ml)
  5. washThe extract was washed with water (100 ml)
  6. dry with materialdried over Na2SO4
  7. customto give a pale yellow oil which
  8. distillationwas distilled under reduced pressure

출처 및 근거

ORD 기록
ord-8ee1f8debc9d451f9013b77fecc83891
출처 데이터셋
uspto-grants-1991_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04988733

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