Hydrochloric Acid → 2-(5-oxo-5H-dibenzo[a,d]cyclohepten-2-yl)propanal oxime

HRID 2072519노트

반응식

HRID 2072519 반응식
[O:1]=[C:2]1[C:8]2[CH:9]=[CH:10][C:11]([CH:13]([CH3:16])[CH:14]=O)=[CH:12][C:7]=2[CH:6]=[CH:5][C:4]2[CH:17]=[CH:18][CH:19]=[CH:20][C:3]1=2.Cl.[NH2:22][OH:23].[OH-].[Na+].Cl>O.C(O)C>[O:1]=[C:2]1[C:8]2[CH:9]=[CH:10][C:11]([CH:13]([CH3:16])[CH:14]=[N:22][OH:23])=[CH:12][C:7]=2[CH:6]=[CH:5][C:4]2[CH:17]=[CH:18][CH:19]=[CH:20][C:3]1=2

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 214093832-(5-oxo-5H-dibenzo[a,d]cyclohepten-2-yl)propanal

생성물 1

HCID 867351132-(5-oxo-5H-dibenzo[a,d]cyclohepten-2-yl)propanal oxime

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

To a solution of 0.288 g. of 2-(5-oxo-5H-dibenzo[a,d]cyclohepten-2-yl)propanal in 4 ml. of ethanol is added a solution of 0.12 g. of hydroxylamine hydrochloride and 0.11 g. of sodium hydroxide in 0.4 ml. of water. The mixture is refluxed briefly, then acidified with dilute hydrochloric acid and extracted with ethyl acetate. The extract is washed, dried and evaporated to yield a crude product which is chromatographed on silica gel, eluting with chloroform:methanol (19:1) to afford 2-(5-oxo-5H-dibenzo[a,d]cyclohepten-2-yl)propanal oxime.

후처리

  1. temperatureThe mixture is refluxed briefly
  2. extractionextracted with ethyl acetate
  3. washThe extract is washed
  4. customdried
  5. customevaporated
  6. customto yield a crude product which
  7. customis chromatographed on silica gel
  8. washeluting with chloroform:methanol (19:1)

출처 및 근거

ORD 기록
ord-9940313b5bd84752ba23d78d396ad60d
출처 데이터셋
uspto-grants-1977_09
특허 번호
US04051260

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