Sodium Hydroxide → HCID 178440146、化合物

HRID 265110ノート

反応式

HRID 265110 の反応式
[OH:1][CH:2]([C:7]1[N:8]=[C:9]([CH2:32][CH2:33][CH3:34])[N:10]([CH2:14][C:15]2[CH:20]=[CH:19][C:18]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=3[C:27]3[NH:31][N:30]=[N:29][N:28]=3)=[CH:17][CH:16]=2)[C:11]=1[C:12]#[N:13])[C:3]([CH3:6])([CH3:5])[CH3:4].[OH-:35].[Na+]>C(O)C>[OH:1][CH:2]([C:7]1[N:8]=[C:9]([CH2:32][CH2:33][CH3:34])[N:10]([CH2:14][C:15]2[CH:20]=[CH:19][C:18]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=3[C:27]3[NH:31][N:30]=[N:29][N:28]=3)=[CH:17][CH:16]=2)[C:11]=1[C:12]([NH2:13])=[O:35])[C:3]([CH3:6])([CH3:4])[CH3:5]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 178440143HCID 178440143、化合物

生成物 1

HCID 178440146HCID 178440146、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 0.70 g of 4-(1-hydroxy-2,2-dimethylpropyl)-2-propyl-1-{4-[2-(tetrazol-5-yl)phenyl]phenyl}methylimidazole-5-carbonitrile [prepared as described in step (c) above] in 14 ml of 1N aqueous sodium hydroxide and 7 ml of ethanol was heated under reflux for 2 hours. At the end of this time, the ethanol in the reaction mixture was removed by evaporation under reduced pressure, and ethyl acetate and 14 ml of 1N aqueous hydrochloric acid were added to the residue. The ethyl acetate layer was separated, dried over anhydrous magnesium sulfate and concentrated by evaporation under reduced pressure, to give 0.45 g of the title compound as a powder, melting at 174°-176° C.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 2 hours
  3. customAt the end of this time, the ethanol in the reaction mixture was removed by evaporation under reduced pressure, and ethyl acetate and 14 ml of 1N aqueous hydrochloric acid
  4. additionwere added to the residue
  5. customThe ethyl acetate layer was separated
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated by evaporation under reduced pressure

出典と根拠

ORDレコード
ord-4f858280b0484108ba93ade5f4b4b809
出典データセット
uspto-grants-1997_07
特許番号
US05646171

反応ノート

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