Lithium Hydroxide → HCID 58277404、化合物

HRID 1949246ノート

反応式

HRID 1949246 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][C:16]([F:19])=[CH:15][CH:14]=3)[N:11]=[C:10]([C:20]([O:22]CC)=[O:21])[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:14]=[CH:15][C:16]([F:19])=[CH:17][CH:18]=3)[N:11]=[C:10]([C:20]([OH:22])=[O:21])[CH:9]=2)[CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 2

HCID 3939Lithium HydroxideHCID 58277448HCID 58277448、化合物

生成物 1

HCID 58277404HCID 58277404、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
50 °C

実験手順

23.9 g (72.8 mmol) of the compound of Example 40A are provided in 100 ml of 1,4-dioxane, 100 ml (200 mmol) of a 2N solution of lithium hydroxide in water are added, and the mixture is stirred at 50° C. 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 dichloromethane, and the organic phase is dried over magnesium sulfate, filtered and concentrated. The residue is stirred in a little diethyl ether, collected by filtration and dried under high vacuum. 22.0 g (100% of theory) of the title compound are obtained.

後処理

  1. concentrationThe mixture is concentrated
  2. additionthe residue is diluted with water
  3. additiona conc. aqueous hydrogen chloride solution is subsequently added until the pH
  4. extractionthe mixture is extracted with dichloromethane
  5. dry with materialthe organic phase is dried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. stirringThe residue is stirred in a little diethyl ether
  9. filtrationcollected by filtration
  10. customdried under high vacuum

出典と根拠

ORDレコード
ord-9f675896e04242b0b6bfeb7cd8e4250e
出典データセット
uspto-grants-2013_03
特許番号
US08399682B2

反応ノート

読み込み中…