Lithium Hydroxide → HCID 58277379、化合物

HRID 1949237ノート

反応式

HRID 1949237 の反応式
[F:1][C:2]1[CH:3]=[C:4]([C:8]2[N:12]([C:13]3[CH:18]=[CH:17][CH:16]=[C:15]([O:19][CH3:20])[CH:14]=3)[N:11]=[C:10]([C:21]([O:23]CC)=[O:22])[CH:9]=2)[CH:5]=[CH:6][CH:7]=1.[OH-].[Li+]>O1CCOCC1.O>[F:1][C:2]1[CH:3]=[C:4]([C:8]2[N:12]([C:13]3[CH:18]=[CH:17][CH:16]=[C:15]([O:19][CH3:20])[CH:14]=3)[N:11]=[C:10]([C:21]([OH:23])=[O:22])[CH:9]=2)[CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 2

HCID 3939Lithium HydroxideHCID 58277408HCID 58277408、化合物

生成物 1

HCID 58277379HCID 58277379、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

反応条件

温度
70 °C

実験手順

34.0 g (99.9 mmol) of the compound of Example 30A are provided in 150 ml of 1,4-dioxane, 150 ml (300 mmol) of a 2N solution of lithium hydroxide in water are added, and the mixture is stirred at 70° C. for 1 h. The mixture is concentrated, a conc. aqueous hydrogen chloride solution is subsequently added to the residue until the pH is acidic, the mixture is extracted with dichloromethane, and the organic phase is dried over magnesium sulfate, filtered and concentrated. The residue is recrystallized from diethyl ether. 26.1 g (84% of theory) of the title compound are obtained.

後処理

  1. concentrationThe mixture is concentrated
  2. additiona conc. aqueous hydrogen chloride solution is subsequently added to the residue until the pH
  3. extractionthe mixture is extracted with dichloromethane
  4. dry with materialthe organic phase is dried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe residue is recrystallized from diethyl ether

出典と根拠

ORDレコード
ord-c89f0417023541f893d3d5423c6797fa
出典データセット
uspto-grants-2013_03
特許番号
US08399682B2

反応ノート

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