Diisopropylethylamine → 6-[4-(5-Fluoro-2-trifluoromethylbenzoyl)piperazin-1-YL]imidazo[1,2-B]pyridazine-2-carboxylic acid ethyl ester

HRID 1985633ノート

反応式

HRID 1985633 の反応式
[CH2:1]([O:3][C:4]([C:6]1[N:7]=[C:8]2[CH:13]=[CH:12][C:11]([N:14]3[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]3)=[N:10][N:9]2[CH:20]=1)=[O:5])[CH3:2].C(N(C(C)C)CC)(C)C.[F:30][C:31]1[CH:32]=[CH:33][C:34]([C:40]([F:43])([F:42])[F:41])=[C:35]([CH:39]=1)[C:36](Cl)=[O:37]>ClCCl>[CH2:1]([O:3][C:4]([C:6]1[N:7]=[C:8]2[CH:13]=[CH:12][C:11]([N:14]3[CH2:19][CH2:18][N:17]([C:36](=[O:37])[C:35]4[CH:39]=[C:31]([F:30])[CH:32]=[CH:33][C:34]=4[C:40]([F:43])([F:41])[F:42])[CH2:16][CH2:15]3)=[N:10][N:9]2[CH:20]=1)=[O:5])[CH3:2]

参加物

5

反応物 3

HCID 81531DiisopropylethylamineHCID 27375605-Fluoro-2-(trifluoromethyl)benzoyl chlorideHCID 668640036-Piperazin-1-ylimidazo[1,2-b]pyridazine-2-carboxylic acid ethyl ester

生成物 1

HCID 668634596-[4-(5-Fluoro-2-trifluoromethylbenzoyl)piperazin-1-YL]imidazo[1,2-B]pyridazine-2-carboxylic acid ethyl ester収率 82%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of 6-piperazin-1-ylimidazo[1,2-b]pyridazine-2-carboxylic acid ethyl ester (1.016 g, 3.69 mmol) and diisopropylethylamine (1.29 mL, 7.38 mmol) in anhydrous dichloromethane (20 mL) was added 5-fluoro-2-trifluoromethylbenzoyl chloride dropwise at room temperature. The reaction mixture was stirred at room temperature for 15 minutes, then diluted with dichloromethane and washed with water. The organic layer was dried and concentrated in vacuo. The title compound was obtained in 82% yield (1.365 g) after purification by column chromatography.

後処理

  1. washwashed with water
  2. customThe organic layer was dried
  3. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-b6abe68b91a44bf38cb5c4c2c28d91ae
出典データセット
uspto-grants-2009_06
特許番号
US07547698B2

反応ノート

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