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Hydrochloric Acid → HCID 11593499, 화합물

HRID 1669353
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HRID 1669353 반응식
[Mg].II.Br[C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([CH:11]=[C:12]([F:14])[F:13])[CH:6]=1.[CH:15](N1CCCCC1)=[O:16].Cl>O1CCCC1>[F:13][C:12]([F:14])=[CH:11][C:7]1[CH:6]=[C:5]([CH:10]=[CH:9][CH:8]=1)[CH:15]=[O:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 807IodineHCID 174291-PiperidinecarboxaldehydeHCID 5462224MagnesiumHCID 113564273-Bromo-beta,beta-difluorostyrene

생성물 1

HCID 11593499HCID 11593499, 화합물수율 24.5%

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매
3회

실험 절차

To a mixture of 0.67 g of magnesium and 10 ml of tetrahydrofuran was added a catalytic amount of iodine, and added dropwise a solution of 6.0 g of 1-bromo-3-(2,2-difluoroethenyl)benzene in 20 ml of tetrahydrofuran at 55° C. After stirred at room temperature for 15 minutes, a solution of 3.98 g of 1-formylpiperidine in 5 ml of tetrahydrofuran was added dropwise. This was heated under reflux for 15 minutes, and ice water and 10% hydrochloric acid were added, followed by extraction with t-butyl methyl ether. The organic layer was washed with an aqueous saturated sodium chloride solution, dried over anhydrous magnesium sulfate and then concentrated. The resulting residue was subjected to silica gel column chromatography to obtained 1.13 g of oily 3-(2,2-difluoroethenyl)benzaldehyde [Compound No. (1)].

후처리

  1. temperatureThis was heated
  2. temperatureunder reflux for 15 minutes
  3. extractionfollowed by extraction with t-butyl methyl ether
  4. washThe organic layer was washed with an aqueous saturated sodium chloride solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-5ac1575064104f53afa1e1d6d162a245
출처 데이터셋
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07989478B2

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