Water → Methyl 2-{[1-(1-naphthyl)-5-(2,6-dimethoxyphenyl)-3-pyrazolyl]carbonylamino}-2-adamantanecarboxylate

HRID 1600080ノート

反応式

HRID 1600080 の反応式
[C:1]1([N:11]2[C:15]([C:16]3[C:21]([O:22][CH3:23])=[CH:20][CH:19]=[CH:18][C:17]=3[O:24][CH3:25])=[CH:14][C:13]([C:26]([NH:28][C:29]3([C:39]([OH:41])=[O:40])[CH:36]4[CH2:37][CH:32]5[CH2:33][CH:34]([CH2:38][CH:30]3[CH2:31]5)[CH2:35]4)=[O:27])=[N:12]2)[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1.O.[C:43](=O)([O-])[O-].[Cs+].[Cs+]>O1CCCC1.CN(C)C=O>[C:1]1([N:11]2[C:15]([C:16]3[C:17]([O:24][CH3:25])=[CH:18][CH:19]=[CH:20][C:21]=3[O:22][CH3:23])=[CH:14][C:13]([C:26]([NH:28][C:29]3([C:39]([O:41][CH3:43])=[O:40])[CH:36]4[CH2:35][CH:34]5[CH2:33][CH:32]([CH2:31][CH:30]3[CH2:38]5)[CH2:37]4)=[O:27])=[N:12]2)[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1

参加物

6

反応物 3

HCID 962WaterHCID 10796Cesium carbonateHCID 189266642-{[1-(1-Naphthyl)-5-(2,6-dimethoxyphenyl)-3-pyrazolyl]carbonylamino}-2-adamantanecarboxylic acid

生成物 1

HCID 18926647Methyl 2-{[1-(1-naphthyl)-5-(2,6-dimethoxyphenyl)-3-pyrazolyl]carbonylamino}-2-adamantanecarboxylate

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

0.5 g of the compound prepared in Example 11 is dissolved in 34.6 ml of anhydrous tetrahydrofuran and 4 ml of dimethylformamide. 3.5 ml of water and 0.208 g of caesium carbonate are added and the reaction mixture is left at room temperature for 1 hour. It is concentrated under vacuum and treated azeotropically with toluene. The residue is taken up in 5 ml of tetrahydrofuran. 0.6 ml of methyl iodide is added and the reaction mixtureis left for 1 hour at room temperature. It is concentrated under vacuum, the residue is taken up in water, the mixture is stirred and the precipitate is separated by filtration. The precipitate is washed with water and with pentane.

後処理

  1. concentrationIt is concentrated under vacuum
  2. additiontreated azeotropically with toluene
  3. addition0.6 ml of methyl iodide is added
  4. waitthe reaction mixtureis left for 1 hour at room temperature
  5. concentrationIt is concentrated under vacuum
  6. customthe precipitate is separated by filtration
  7. washThe precipitate is washed with water and with pentane

出典と根拠

ORDレコード
ord-1d8ce1c0c7324c94a19faec104aef7da
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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