Lithium Hydroxide → HCID 58277404, 화합물

HRID 1949246노트

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HRID 1949246 반응식
[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

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 58277448HCID 58277448, 화합물

생성물 1

HCID 58277404HCID 58277404, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매

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온도
50 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9f675896e04242b0b6bfeb7cd8e4250e
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08399682B2

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