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

HRID 17890ノート

反応式

HRID 17890 の反応式
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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
70 °C

実験手順

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,

後処理

  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)

出典と根拠

ORDレコード
ord-aa319d98b94f435396b145547cac0460
出典データセット
uspto-grants-2010_06
特許番号
US07741323B2

反応ノート

読み込み中…