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Trifluoroacetic acid → 1-[5-({[5-methyl 1-(4-methylphenyl)-1H-pyrazol-4-yl]carbonyl}amino)pyridin-2-yl]-4-oxocyclohexanecarboxylic acid ethyl ester

HRID 1748636
ノート
印刷プレビュー

反応式

HRID 1748636 の反応式
FC(F)(F)C(O)=O.[CH2:8]([O:10][C:11]([C:13]1([C:23]2[CH:28]=[CH:27][C:26]([NH:29][C:30]([C:32]3[CH:33]=[N:34][N:35]([C:38]4[CH:43]=[CH:42][C:41]([CH3:44])=[CH:40][CH:39]=4)[C:36]=3[CH3:37])=[O:31])=[CH:25][N:24]=2)[CH2:22][CH2:21][C:16]2(OCC[O:17]2)[CH2:15][CH2:14]1)=[O:12])[CH3:9]>ClCCl>[CH2:8]([O:10][C:11]([C:13]1([C:23]2[CH:28]=[CH:27][C:26]([NH:29][C:30]([C:32]3[CH:33]=[N:34][N:35]([C:38]4[CH:39]=[CH:40][C:41]([CH3:44])=[CH:42][CH:43]=4)[C:36]=3[CH3:37])=[O:31])=[CH:25][N:24]=2)[CH2:22][CH2:21][C:16](=[O:17])[CH2:15][CH2:14]1)=[O:12])[CH3:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6422Trifluoroacetic acid2 回HCID 866925638-[5-({[5-Methyl-1-(4-methylphenyl)-1H-pyrazol-4-yl]carbonyl}amino)pyridin-2-yl]-1,4-dioxaspiro[4.5]decane-8-carboxylic acid ethyl ester

生成物 1

HCID 866925731-[5-({[5-methyl 1-(4-methylphenyl)-1H-pyrazol-4-yl]carbonyl}amino)pyridin-2-yl]-4-oxocyclohexanecarboxylic acid ethyl ester収率 94%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Trifluoroacetic acid (0.96 ml) was added at room temperature to a solution of 8-[5-({[5-methyl-1-(4-methylphenyl)-1H-pyrazol-4-yl]carbonyl}amino)pyridin-2-yl]-1,4-dioxaspiro[4.5]decane-8-carboxylic acid ethyl ester (1.27 g) described in Example D4 in dichloromethane (2.5 ml) and stirred at the same temperature for six hours. Trifluoroacetic acid (1.9 ml) was added at the same temperature and stirred at the same temperature for 18 hours. After the reaction, the solvent and trifluoroacetic acid were evaporated, a saturated aqueous solution of sodium bicarbonate was added and extracted with ethyl acetate twice. The organic solution was dried over anhydrous magnesium sulfate and concentrated to give 1-[5-({[5-methyl 1-(4-methylphenyl)-1H-pyrazol-4-yl]carbonyl}amino)pyridin-2-yl]-4-oxocyclohexanecarboxylic acid ethyl ester (1.09 g) as a white solid.

後処理

  1. stirringstirred at the same temperature for 18 hours
  2. customAfter the reaction
  3. customthe solvent and trifluoroacetic acid were evaporated
  4. additiona saturated aqueous solution of sodium bicarbonate was added
  5. extractionextracted with ethyl acetate twice
  6. dry with materialThe organic solution was dried over anhydrous magnesium sulfate
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-3e39cfae10ee4b959e0ee0fdb6300bc9
出典データセット
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09150555B2

反応ノート

読み込み中…

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