Hydrochloric Acid → 2-{[1-(1-Naphthyl)-5-(2,6-dimethoxyphenyl)-3-pyrazolyl]carbonylamino}-2-adamantanecarboxylic acid

HRID 1600079ノート

反応式

HRID 1600079 の反応式
[OH-].[Na+].[NH2:3][C:4]1([C:14]([OH:16])=[O:15])[CH:11]2[CH2:12][CH:7]3[CH2:8][CH:9]([CH2:13][CH:5]1[CH2:6]3)[CH2:10]2.[C:17]1([N:27]2[C:31]([C:32]3[C:37]([O:38][CH3:39])=[CH:36][CH:35]=[CH:34][C:33]=3[O:40][CH3:41])=[CH:30][C:29]([C:42](Cl)=[O:43])=[N:28]2)[C:26]2[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=2)[CH:20]=[CH:19][CH:18]=1.Cl>O.O1CCCC1>[C:17]1([N:27]2[C:31]([C:32]3[C:37]([O:38][CH3:39])=[CH:36][CH:35]=[CH:34][C:33]=3[O:40][CH3:41])=[CH:30][C:29]([C:42]([NH:3][C:4]3([C:14]([OH:16])=[O:15])[CH:11]4[CH2:10][CH:9]5[CH2:8][CH:7]([CH2:6][CH:5]3[CH2:13]5)[CH2:12]4)=[O:43])=[N:28]2)[C:26]2[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=2)[CH:20]=[CH:19][CH:18]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 14798Sodium Hydroxide2 回HCID 643542-Aminoadamantane-2-carboxylic acidHCID 189266441-(1-Naphthyl)-5-(2,6-dimethoxyphenyl)-3-pyrazolecarbonyl chloride

生成物 1

HCID 189266642-{[1-(1-Naphthyl)-5-(2,6-dimethoxyphenyl)-3-pyrazolyl]carbonylamino}-2-adamantanecarboxylic acid

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒3 回

実験手順

0.107 g of sodium hydroxide in 1.36 ml of water and 0.51 ml of tetrahydrofuran are cooled to 0° C. 0.52 g of 2-amino-2-adamantanecarboxylic acid is added in a single portion, and 0.53g of 1-(1-naphthyl)-5-(2,6-dimethoxyphenyl)-3-pyrazolecarbonyl chloride, dissolved in 3 ml of tetrahydrofuran, is then added dropwise. The mixture is left for 10 minutes, and the same amount of the above acid chloride, in3 ml of tetrahydrofuran, is added again; simultaneously, 1.32 ml of 2N sodium hydroxide are added. The reaction mixture is left for 4 days at room temperature; successively, ice-cold water is added and concentrated hydrochloric acid is added to pH 1, and the precipitate is filtered off. The crystals are washed with diisopropyl ether.

後処理

  1. additionis then added dropwise
  2. waitThe reaction mixture is left for 4 days at room temperature
  3. additionsuccessively, ice-cold water is added
  4. filtrationthe precipitate is filtered off
  5. washThe crystals are washed with diisopropyl ether

出典と根拠

ORDレコード
ord-4fdb9758c51e4ee08c9427660add9fea
出典データセット
uspto-grants-1998_04
特許番号
US05744491

反応ノート

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