Lithium Hydroxide → HCID 58277379, 화합물

HRID 1949237노트

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HRID 1949237 반응식
[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

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 58277408HCID 58277408, 화합물

생성물 1

HCID 58277379HCID 58277379, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매

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온도
70 °C

실험 절차

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.

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
  7. customThe residue is recrystallized from diethyl ether

출처 및 근거

ORD 기록
ord-c89f0417023541f893d3d5423c6797fa
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08399682B2

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