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Water → 1-(4-chlorophenyl)-8,9-dihydro-7-methylene-7H-pyrrolo[3,2,1-ij]quinoline

HRID 263426
ノート
印刷プレビュー

反応式

HRID 263426 の反応式
[CH3:1]C(C)([O-])C.[K+].[Cl:7][C:8]1[CH:13]=[CH:12][C:11]([C:14]2[C:24]3=[C:25]4[C:20]([C:21](=O)[CH2:22][CH2:23]3)=[CH:19][CH:18]=[CH:17][N:16]4[CH:15]=2)=[CH:10][CH:9]=1.O>[Br-].C[P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.O1CCCC1>[Cl:7][C:8]1[CH:13]=[CH:12][C:11]([C:14]2[C:24]3=[C:25]4[C:20]([C:21](=[CH2:1])[CH2:22][CH2:23]3)=[CH:19][CH:18]=[CH:17][N:16]4[CH:15]=2)=[CH:10][CH:9]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 962WaterHCID 190380211-(4-chlorophenyl)-8,9-dihydro-7H-pyrrolo[3,2,1-ij]quinolin-7-oneHCID 23665647Potassium tert-butoxide

生成物 1

HCID 190380201-(4-chlorophenyl)-8,9-dihydro-7-methylene-7H-pyrrolo[3,2,1-ij]quinoline

試薬・触媒・溶媒 2

HCID 74505Methyltriphenyliphosphonium bromide触媒
HCID 8028
Tetrahydrofuran
溶媒
3 回

実験手順

Methyltriphenylphosphonium bromide (3.8 g) was added to 25 ml of anhydrous tetrahydrofuran. To this mixture was added the solution of potassium t-butoxide (1.2 g) in 25 ml of tetrahydrofuran at ambient temperature. After stirring for 3 hours, to this solution was added the solution of 1-(4-chlorophenyl)-8,9-dihydro-7H-pyrrolo[3,2,1-ij]quinolin-7-one (1.5 g), which was obtained in example 2, in 15 ml of tetrahydrofuran. After stirring for 30 min., to this solution was added water and extracted with ethyl acetate. The organic solution was washed with brine and dried over anhydrous sodium sulfate. After removing drying agent by filtration and organic solvent by evaporation under reduced pressure, the residue was purified by alumina column chromatography, and the title compound was obtained as yellow crystals (1.1 g) .

後処理

  1. stirringAfter stirring for 30 min., to this solution
  2. extractionextracted with ethyl acetate
  3. washThe organic solution was washed with brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. customAfter removing
  6. customdrying agent
  7. filtrationby filtration and organic solvent
  8. customby evaporation under reduced pressure
  9. customthe residue was purified by alumina column chromatography

出典と根拠

ORDレコード
ord-35a96525160248209cc22e79df0949ea
出典データセット
uspto-grants-1997_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05643920

反応ノート

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