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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Lithium Hydroxide → HCID 58277359, 화합물

HRID 1949243
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HRID 1949243 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([N:8]2[C:12]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=3[F:19])=[CH:11][C:10]([C:20]([O:22]CC)=[O:21])=[N:9]2)[CH:5]=[CH:6][CH:7]=1.O1CCOCC1.[OH-].[Li+]>O>[Cl:1][C:2]1[CH:3]=[C:4]([N:8]2[C:12]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=3[F:19])=[CH:11][C:10]([C:20]([OH:22])=[O:21])=[N:9]2)[CH:5]=[CH:6][CH:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 3939Lithium HydroxideHCID 312751,4-DioxaneHCID 58277383HCID 58277383, 화합물

생성물 1

HCID 58277359HCID 58277359, 화합물

시약·촉매·용매 1

HCID 962Water용매2회

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온도
50 °C

실험 절차

2.30 g (6.67 mmol) of the compound of Example 36A are provided in 32 ml of a 2:1 mixture of 1,4-dioxane and water, 17 ml (33.4 mmol) of a 2N solution of lithium hydroxide in water are added, and the mixture is stirred at 50° C. for 2 h. The mixture is concentrated, a 2N aqueous hydrogen chloride solution is subsequently added to the residue until the pH is acidic, the mixture is extracted with ethyl acetate, and the organic phase is dried over sodium sulfate, filtered and concentrated. The residue is stirred in a little of a mixture of petroleum ether and diethyl ether, collected by filtration and dried under high vacuum. 1.58 g (75% of theory) of the title compound are obtained.

후처리

  1. additionare added
  2. concentrationThe mixture is concentrated
  3. additiona 2N aqueous hydrogen chloride solution is subsequently added to the residue until the pH
  4. extractionthe mixture is extracted with ethyl acetate
  5. dry with materialthe organic phase is dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. stirringThe residue is stirred in a
  9. additionlittle of a mixture of petroleum ether and diethyl ether
  10. filtrationcollected by filtration
  11. customdried under high vacuum

출처 및 근거

ORD 기록
ord-0abd0e1c8f70485c8216af71f36f9376
출처 데이터셋
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08399682B2

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