Hydrochloric Acid → 2-Cyano-2-(3,4-dichloro-5(2H)-oxo-2-furyl)acetamide

HRID 447798

반응식

HRID 447798 반응식
[C:1]([OH:9])(=O)/[C:2](=[C:4](\[CH:6]=[O:7])/[Cl:5])/[Cl:3].[C:10]([CH2:12][C:13]([NH2:15])=[O:14])#[N:11].[OH-].[Na+].Cl>CO>[C:10]([CH:12]([CH:1]1[C:2]([Cl:3])=[C:4]([Cl:5])[C:6](=[O:7])[O:9]1)[C:13]([NH2:15])=[O:14])#[N:11]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 7898CyanoacetamideHCID 14798Sodium HydroxideHCID 2771871Mucochloric Acid

생성물 1

HCID 5417922-Cyano-2-(3,4-dichloro-5(2H)-oxo-2-furyl)acetamide수율 17.8%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

Mucochloric acid (15.1 g) and 2-cyanoacetamide (7.53 g) were dissolved in methanol (53.6 ml), and 2.5N aqueous sodium hydroxide solution (53.6 ml) was added dropwise with stirring under ice-cooling. The mixture was allowed to warm to room temperature, and further stirred at room temperature for 3 hr. The reaction mixture was poured into 1N hydrochloric acid containing ice water, methanol was evaporated under reduced pressure, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was crystallized from ethanol-diisopropyl ether to give the title compound (3.74 g) as pale-brown crystals.

후처리

  1. temperaturecooling
  2. stirringfurther stirred at room temperature for 3 hr
  3. customwas evaporated under reduced pressure
  4. extractionthe mixture was extracted with ethyl acetate
  5. washThe extract was washed with saturated brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customThe solvent was evaporated under reduced pressure
  8. customThe residue was crystallized from ethanol-diisopropyl ether

출처 및 근거

ORD 기록
ord-cf68c47ef71349c1880e6365e5ca62c0
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08481569B2

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