Hydrochloric Acid → HCID 82780306、化合物

HRID 2096792ノート

反応式

HRID 2096792 の反応式
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

参加物

6

反応物 4

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

生成物 1

HCID 82780306HCID 82780306、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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+].

後処理

  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)

出典と根拠

ORDレコード
ord-a058e267bba245418fd1769c0996749e
出典データセット
uspto-grants-2013_05
特許番号
US08450313B2

反応ノート

読み込み中…