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Lithium Hydroxide → HCID 58277417、化合物

HRID 1949234
ノート
印刷プレビュー

反応式

HRID 1949234 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([N:8]2[C:12]([C:13]3[CH:18]=[CH:17][C:16]([F:19])=[C:15]([C:20]([F:23])([F:22])[F:21])[CH:14]=3)=[CH:11][C:10]([C:24]([O:26]CC)=[O:25])=[N:9]2)[CH:5]=[CH:6][CH:7]=1.[OH-].[Li+]>O1CCOCC1.O>[Cl:1][C:2]1[CH:3]=[C:4]([N:8]2[C:12]([C:13]3[CH:18]=[CH:17][C:16]([F:19])=[C:15]([C:20]([F:22])([F:23])[F:21])[CH:14]=3)=[CH:11][C:10]([C:24]([OH:26])=[O:25])=[N:9]2)[CH:5]=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 3939Lithium HydroxideHCID 58277455HCID 58277455、化合物

生成物 1

HCID 58277417HCID 58277417、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

実験手順

3.60 g (8.72 mmol) of the compound of Example 27A are provided in 50 ml of 1,4-dioxane, 50 ml (50 mmol) of a 1N solution of lithium hydroxide in water are added, and the mixture is heated under reflux for 1 h. The mixture is concentrated, the residue is diluted with water, a conc. aqueous hydrogen chloride solution is subsequently added until the pH is acidic, the mixture is extracted with ethyl acetate, and the organic phase is dried over magnesium sulfate, filtered and concentrated. 3.30 g (98% of theory) of the title compound are obtained.

後処理

  1. temperaturethe mixture is heated
  2. temperatureunder reflux for 1 h
  3. concentrationThe mixture is concentrated
  4. additionthe residue is diluted with water
  5. additiona conc. aqueous hydrogen chloride solution is subsequently added until the pH
  6. extractionthe mixture is extracted with ethyl acetate
  7. dry with materialthe organic phase is dried over magnesium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated

出典と根拠

ORDレコード
ord-a5d98e00d8bc4a9d9f381666a1a8d71c
出典データセット
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08399682B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート