Dichloromethane → 1-(2-Methylphenyl)-6-methylpyrrolo[3,2-c]cinnoline

HRID 704573

反応式

HRID 704573 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N:8]1[C:20]2[C:19]3[CH:18]=[CH:17][CH:16]=[C:15]([CH3:21])[C:14]=3[N:13]=[N:12][C:11]=2[CH2:10][CH2:9]1.ClCCl>C1(OC2C=CC=CC=2)C=CC=CC=1.C(Cl)(Cl)Cl.[Pd]>[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N:8]1[C:20]2[C:19]3[CH:18]=[CH:17][CH:16]=[C:15]([CH3:21])[C:14]=3[N:13]=[N:12][C:11]=2[CH:10]=[CH:9]1

参加物

6

反応物 2

HCID 6344DichloromethaneHCID 200727571-(2-Methylphenyl)-6-methyl-2,3-dihydropyrrolo [3,2-c]cinnoline

生成物 1

HCID 200727541-(2-Methylphenyl)-6-methylpyrrolo[3,2-c]cinnoline

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 6212Chloroform溶媒2 回HCID 7583Diphenyl Ether溶媒

実験手順

To a refluxing slurry of 10% Pd/C (0.4 g) in diphenyl ether (20 ml) was added 1-(2-methylphenyl)-6-methyl-2,3-dihydropyrrolo [3,2-c]cinnoline (1.25 g, 0.0045 mol). After 0.5 hour at reflux temperature the reaction mixture was cooled, diluted with chloroform and the catalyst was filtered off over hyflo. The product was isolated by column chromatography using dichloromethane (11) then chloroform. The oil obtained was crystallized from ethyl acetate, 0.42 g, m.p. 105-106°.

後処理

  1. temperatureAfter 0.5 hour at reflux temperature the reaction mixture
  2. temperaturewas cooled
  3. filtrationthe catalyst was filtered off over hyflo
  4. customThe product was isolated by column chromatography
  5. customThe oil obtained
  6. customwas crystallized from ethyl acetate, 0.42 g, m.p. 105-106°

出典と根拠

ORDレコード
ord-c6ddbe0469dc4c2e99913a8c9ed2a0f2
出典データセット
uspto-grants-1991_01
特許番号
US04988695

関連ノート

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