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Sodium Hydroxide → 3-(3-Chloropyridazin-6-yl)-2-phenylpyrazolo[1,5-a]pyridine

HRID 276924
ノート
印刷プレビュー

反応式

HRID 276924 の反応式
[Cl:1][C:2]1[N:7]=[N:6][C:5]([C:8]#[C:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[CH:4][CH:3]=1.[C:16]1([C:22]#[C:23][C:24]2[N:25]=[N:26][C:27]([C:30]#[C:31][C:32]3[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=3)=[CH:28][CH:29]=2)[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.[I-].[NH2:39][N+:40]1[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=1.[OH-].[Na+]>[Cl-].C([N+](C)(C)C)C1C=CC=CC=1.ClCCl.O>[Cl:1][C:2]1[N:7]=[N:6][C:5]([C:8]2[C:9]([C:10]3[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=3)=[N:26][N:25]3[CH:24]=[CH:23][CH:22]=[CH:16][C:21]=23)=[CH:4][CH:3]=1.[C:16]1([C:22]#[C:23][C:24]2[N:25]=[N:26][C:27]([C:30]3[C:31]([C:32]4[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=4)=[N:39][N:40]4[CH:45]=[CH:44][CH:43]=[CH:42][C:41]=34)=[CH:28][CH:29]=2)[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 4

HCID 14798Sodium HydroxideHCID 2733704Pyridinium, 1-amino-, iodide (1:1)HCID 126802603-Chloro-6-(phenylethynyl)pyridazineHCID 126802613,6-Bis(2-phenylethynyl)pyridazine

生成物 2

HCID 151581443-(3-Chloropyridazin-6-yl)-2-phenylpyrazolo[1,5-a]pyridineHCID 22629223
3-[3-(2-Phenylethynyl)pyridazin-6-yl]-2-phenylpyrazolo[1,5-a]pyridine

試薬・触媒・溶媒 3

HCID 5963Benzyltrimethylammonium chloride触媒HCID 962Water溶媒2 回HCID 6344Dichloromethane溶媒2 回

実験手順

A 4:1 mixture of 6-chloro-3-(2-phenylethynyl)pyridazine and 3,6-bis(2-phenylethynyl)pyridazine (10.2 g) was stirred in a two-phase mixture of N-aminopyridinium iodide (90% purity; 11 g), benzyltrimethylammonium chloride (1.4 g), sodium hydroxide (5.9 g), dichloromethane (51 ml), and water (51 ml) at ambient temperature for an hour. The reaction mixture was diluted with dichloromethane and water. The organic layer was separated, and the aqueous layer was extracted once with dichloromethane. The combined organic layer was washed with water and brine, dried over anhydrous magnesium sulfate, and concentrated in vacuo. The residue was subjected to column chromatography on silica gel (elution with 25:1 dichloromethane-ethyl acetate) to give 3-(3-chloropyridazin-6-yl)-2-phenylpyrazolo[1,5-a]pyridine (0.72 g) and 3-[3-(2-phenylethynyl)pyridazin-6-yl]-2-phenylpyrazolo[1,5-a]pyridine (0.5 g). Some fractions containing the mixture thereof were subjected to flash column chromatography on silica gel (elution with 50:1 dichloromethane-ethyl acetate) gave an additional product of 3-(3-chloropyridazin-6-yl)-2-phenylpyrazolo[1,5-a]pyridine (0.34 g) and 3-[3-(2-phenylethynyl)pyridazin-6-yl]-2-phenylpyrazolo[1,5-a]pyridine (0.50 g).

後処理

  1. customThe organic layer was separated
  2. extractionthe aqueous layer was extracted once with dichloromethane
  3. washThe combined organic layer was washed with water and brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-e9c6de11ff9c4910a215abf7d7cb93d0
出典データセット
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06355640B1

反応ノート

読み込み中…

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