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Lithium Hydroxide → HCID 58277359、化合物

HRID 1949243
ノート
印刷プレビュー

反応式

HRID 1949243 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][CH:16]=[CH:15][C:14]=3[F:19])=[CH:11][C:10]([C:20]([O:22]CC)=[O:21])=[N:9]2)[CH:5]=[CH:6][CH:7]=1.O1CCOCC1.[OH-].[Li+]>O>[Cl:1][C:2]1[CH:3]=[C:4]([N:8]2[C:12]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=3[F:19])=[CH:11][C:10]([C:20]([OH:22])=[O:21])=[N:9]2)[CH:5]=[CH:6][CH:7]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 3939Lithium HydroxideHCID 312751,4-DioxaneHCID 58277383HCID 58277383、化合物

生成物 1

HCID 58277359HCID 58277359、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
50 °C

実験手順

2.30 g (6.67 mmol) of the compound of Example 36A are provided in 32 ml of a 2:1 mixture of 1,4-dioxane and water, 17 ml (33.4 mmol) of a 2N solution of lithium hydroxide in water are added, and the mixture is stirred at 50° C. for 2 h. The mixture is concentrated, a 2N aqueous hydrogen chloride solution is subsequently added to the residue until the pH is acidic, the mixture is extracted with ethyl acetate, and the organic phase is dried over sodium sulfate, filtered and concentrated. The residue is stirred in a little of a mixture of petroleum ether and diethyl ether, collected by filtration and dried under high vacuum. 1.58 g (75% of theory) of the title compound are obtained.

後処理

  1. additionare added
  2. concentrationThe mixture is concentrated
  3. additiona 2N aqueous hydrogen chloride solution is subsequently added to the residue until the pH
  4. extractionthe mixture is extracted with ethyl acetate
  5. dry with materialthe organic phase is dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. stirringThe residue is stirred in a
  9. additionlittle of a mixture of petroleum ether and diethyl ether
  10. filtrationcollected by filtration
  11. customdried under high vacuum

出典と根拠

ORDレコード
ord-0abd0e1c8f70485c8216af71f36f9376
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

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