Hydrochloric Acid → HCID 82780306, 화합물

HRID 2386781노트

반응식

HRID 2386781 반응식
CC(C)([O-])C.[K+].[CH3:7][C:8]([C:10]1[CH:15]=[CH:14][C:13]([Br:16])=[CH:12][C:11]=1[Cl:17])=O.Cl.[C:19]([O-:22])(O)=O.[Na+]>C1COCC1>[Br:16][C:13]1[CH:14]=[CH:15][C:10]([CH:8]([CH3:7])[CH:19]=[O:22])=[C:11]([Cl:17])[CH:12]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 155609501-(4-Bromo-2-chlorophenyl)ethan-1-oneHCID 23665647Potassium tert-butoxide

생성물 1

HCID 82780306HCID 82780306, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Potassium tert-butoxide (7.53 g) was added to a solution 2-chloro-4-bromoacetophenone (CAS Reg. No. 252561-81-2, 10.45 g) and (methoxymethyl)-triphenylphosphosium chloride (21.48 g) in THF (100 ml) at room temperature. The mixture was stirred for 1 h at room temperature. 25% aqueous HCl (90 ml) was added. The resulting mixture was stirred 1 h at room temperature and poured then carefully to a saturated aqueous NaHCO3 solution. After neutralization, the mixture was extracted with EtOAc. The combined organic layers were dried over Na2SO4 and then concentrated to an oil. The residue was purified by flash chromatography (SiO2, EtOAc/heptane 1:4) to give the title compound (8.1 g) as a yellow oil. MS (m/e, ISP neg. ion)=247.2 [M−H+].

후처리

  1. customat room temperature
  2. stirringThe resulting mixture was stirred 1 h at room temperature
  3. additionpoured
  4. extractionAfter neutralization, the mixture was extracted with EtOAc
  5. dry with materialThe combined organic layers were dried over Na2SO4
  6. concentrationconcentrated to an oil
  7. customThe residue was purified by flash chromatography (SiO2, EtOAc/heptane 1:4)

출처 및 근거

ORD 기록
ord-a4a14afcfcf247869a5502da8ecd7ea3
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08268820B2

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