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Acetic Acid → N-[6-(1-Cyano-4-oxocyclohexyl)pyridin-3-yl]-5-methyl-1-(4-methylphenyl)-1H-pyrazole-4-carboxamide

HRID 1748639
ノート
印刷プレビュー

反応式

HRID 1748639 の反応式
[C:1]([C:3]1([C:13]2[N:18]=[CH:17][C:16]([NH:19][C:20]([C:22]3[CH:23]=[N:24][N:25]([C:28]4[CH:33]=[CH:32][C:31]([CH3:34])=[CH:30][CH:29]=4)[C:26]=3[CH3:27])=[O:21])=[CH:15][CH:14]=2)[CH2:12][CH2:11][C:6]2(OCC[O:7]2)[CH2:5][CH2:4]1)#[N:2].C(O)(=O)C.Cl.C(=O)([O-])[O-].[K+].[K+]>O>[C:1]([C:3]1([C:13]2[N:18]=[CH:17][C:16]([NH:19][C:20]([C:22]3[CH:23]=[N:24][N:25]([C:28]4[CH:29]=[CH:30][C:31]([CH3:34])=[CH:32][CH:33]=4)[C:26]=3[CH3:27])=[O:21])=[CH:15][CH:14]=2)[CH2:12][CH2:11][C:6](=[O:7])[CH2:5][CH2:4]1)#[N:2]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 86692570HCID 86692570、化合物

生成物 1

HCID 86692577N-[6-(1-Cyano-4-oxocyclohexyl)pyridin-3-yl]-5-methyl-1-(4-methylphenyl)-1H-pyrazole-4-carboxamide収率 58.7%

試薬・触媒・溶媒 1

HCID 962
Water
溶媒

反応条件

温度
100 °C

実験手順

A solution of N-[6-(8-cyano-1,4-dioxaspiro[4.5]dec-8-yl)pyridin-3-yl]-5-methyl-1-(4-methylphenyl)-1H-pyrazole-4-carboxamide (181 mg) described in Example E3 in a mixed solvent of acetic acid (2 ml), water (0.5 ml) and 1N hydrochloric acid aqueous solution (0.5 ml) was stirred at 100° C. for two hours. After the reaction, a saturated aqueous solution of potassium carbonate was added and extracted with ethyl acetate. The organic solution was dried over anhydrous magnesium sulfate and concentrated. The residue was purified with a column chromatography to give the titled compound (96 mg).

後処理

  1. customAfter the reaction
  2. extractionextracted with ethyl acetate
  3. dry with materialThe organic solution was dried over anhydrous magnesium sulfate
  4. concentrationconcentrated
  5. customThe residue was purified with a column chromatography

出典と根拠

ORDレコード
ord-bb05805260314071b7ba79f224985793
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…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート