Hydrochloric Acid → HCID 14937509, 화합물

HRID 1012377노트

반응식

HRID 1012377 반응식
[C:1]([CH:3]([CH2:9][C:10](=O)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)[C:4]([O:6][CH2:7][CH3:8])=[O:5])#[N:2].[ClH:18]>O1CCCC1>[Cl:18][C:1]1[NH:2][C:10]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[CH:9][C:3]=1[C:4]([O:6][CH2:7][CH3:8])=[O:5]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 15633746Ethyl 2-cyano-4-oxo-4-phenylbutanoate

생성물 1

HCID 14937509HCID 14937509, 화합물수율 79%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution (60 mL) of ethyl 2-cyano-4-oxo-4-phenylbutanoate (5.0 g) in tetrahydrofuran was blown in hydrogen chloride (28 g) under ice-cooling, and the mixture was stirred at room temperature for 3 hr. Then, nitrogen was blown in to remove excess hydrogen chloride. The reaction mixture was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (eluent:hexane-ethyl acetate=6:1) to give the title compound as a pale-yellow solid (yield 4.24 g, 79%).

후처리

  1. temperaturecooling
  2. customto remove excess hydrogen chloride
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. customthe residue was purified by silica gel column chromatography (eluent:hexane-ethyl acetate=6:1)

출처 및 근거

ORD 기록
ord-4cef9a546e414dfe96d5ef9e28bb1353
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07977488B2

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