Lithium Hydroxide → HCID 58277349, 화합물

HRID 1949261노트

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HRID 1949261 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:12]([C:13]3[CH:18]=[CH:17][CH:16]=[C:15]([F:19])[CH:14]=3)=[CH:11][C:10]([C:20]([O:22]CC)=[O:21])=[N:9]2)=[CH:4][CH:3]=1.[OH-].[Li+]>O1CCOCC1.O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([N:8]2[C:12]([C:13]3[CH:18]=[CH:17][CH:16]=[C:15]([F:19])[CH:14]=3)=[CH:11][C:10]([C:20]([OH:22])=[O:21])=[N:9]2)=[CH:6][CH:7]=1

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 58277374HCID 58277374, 화합물

생성물 1

HCID 58277349HCID 58277349, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매

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온도
70 °C

실험 절차

43.0 g (125 mmol) of the compound of Example 56A are provided in 504 ml of 1,4-dioxane, 94 ml (188 mmol) of a 2N solution of lithium hydroxide in water are added, and the mixture is stirred at 70° C. for 2 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. 39.5 g (100% of theory) of the title compound are obtained.

후처리

  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

출처 및 근거

ORD 기록
ord-5764eda8dbbf4ced87049dba07f69fa6
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08399682B2

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