Lithium Hydroxide → HCID 58277445, 화합물

HRID 1949233노트

반응식

HRID 1949233 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([N:8]2[C:12]([C:13]3[CH:18]=[CH:17][CH:16]=[C:15]([O:19][C:20]([F:23])([F:22])[F:21])[CH:14]=3)=[CH:11][C:10]([C:24]([O:26]CC)=[O:25])=[N:9]2)[CH:5]=[CH:6][CH:7]=1.[OH-].[Li+]>O1CCOCC1.O>[Cl:1][C:2]1[CH:3]=[C:4]([N:8]2[C:12]([C:13]3[CH:18]=[CH:17][CH:16]=[C:15]([O:19][C:20]([F:23])([F:22])[F:21])[CH:14]=3)=[CH:11][C:10]([C:24]([OH:26])=[O:25])=[N:9]2)[CH:5]=[CH:6][CH:7]=1

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 58277354HCID 58277354, 화합물

생성물 1

HCID 58277445HCID 58277445, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매

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온도
70 °C

실험 절차

10.8 g (26.2 mmol) of the compound of Example 26A are provided in 236 ml of 1,4-dioxane, 236 ml (472 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 and a 2N 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. 9.90 g (99% of theory) of the title compound are obtained.

후처리

  1. concentrationThe mixture is concentrated
  2. additiona 2N 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-111042a3a74b424baf74afc6488435fc
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08399682B2

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