Hydrochloric Acid → 1-hydroxyimino-3-phenyl-6-(3-phenyl-propoxy)-1H-indene-2-carbonitrile

HRID 17890

반응식

HRID 17890 반응식
O=[C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([O:11][CH2:12][CH2:13][CH2:14][C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)[CH:9]=2)[C:4]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)=[C:3]1[C:27]#[N:28].[OH:29][NH2:30].Cl.N1C=CC=CC=1>C(O)C>[OH:29][N:30]=[C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([O:11][CH2:12][CH2:13][CH2:14][C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)[CH:9]=2)[C:4]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)=[C:3]1[C:27]#[N:28]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 787HydroxylamineHCID 1049PyridineHCID 686950891-oxo-3-phenyl-6-(3-phenylpropoxy)-1H-indene-2-carbonitrile

생성물 1

HCID 866140311-hydroxyimino-3-phenyl-6-(3-phenyl-propoxy)-1H-indene-2-carbonitrile수율 45%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
70 °C

실험 절차

1-Oxo-3-phenyl-6-(3-phenylpropoxy)-1H-indene-2-carbonitrile (200 mg, 0.547 mmol) was dissolved in ethanol. Hydroxy amine.hydrochloric acid (114 mg, 1.64 mmol) and pyridine (173 mg, 2.18 mmol) were added thereto and the mixture was stirred for 4 hours at 70° C. The organic layer extracted with ethyl acetate was washed with distilled water, dried over anhydrous magnesium sulfate, concentrated, and the resulting residue was purified by column chromatography (ethyl acetate:hexane=1:2) to obtain trails 1-hydroxy imino-3-phenyl-6-(3-phenylpropyloxy)-1H-indene-2-carbonitrile (95 mg, yield 45%) as a red solid,

후처리

  1. extractionThe organic layer extracted with ethyl acetate
  2. washwas washed with distilled water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated
  5. customthe resulting residue was purified by column chromatography (ethyl acetate:hexane=1:2)

출처 및 근거

ORD 기록
ord-aa319d98b94f435396b145547cac0460
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07741323B2

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