Lithium Hydroxide → HCID 57436798, 화합물

HRID 2059897노트

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HRID 2059897 반응식
[OH-].[Li+].[F:3][C:4]([F:26])([F:25])[C:5]1[CH:6]=[C:7]([S:11]([N:14]2[CH2:19][CH2:18][CH2:17][CH2:16][CH:15]2[CH2:20][C:21]([O:23]C)=[O:22])(=[O:13])=[O:12])[CH:8]=[CH:9][CH:10]=1>O.O1CCCC1>[F:26][C:4]([F:3])([F:25])[C:5]1[CH:6]=[C:7]([S:11]([N:14]2[CH2:19][CH2:18][CH2:17][CH2:16][CH:15]2[CH2:20][C:21]([OH:23])=[O:22])(=[O:13])=[O:12])[CH:8]=[CH:9][CH:10]=1

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 58711709HCID 58711709, 화합물

생성물 1

HCID 57436798HCID 57436798, 화합물수율 90%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

반응 조건

온도
0 °C

실험 절차

A solution of lithium hydroxide (1 g, 22 mmol) in water (44 ml) was added dropwise to a solution of methyl 2-(1-(3-(trifluoromethyl)phenylsulfonyl)piperidin-2-yl)acetate (4.38 g, 12 mmol) in tetrahydrofuran (176 ml) while stirring at 0° C. The mixture was stirred for 16 h at 25° C. The solvent was removed under vacuum, the residue dissolved in water and washed with diethyl ether. The aqueous phase was carefully acidified with citric acid solution (10%) and extracted with ethyl acetate. This organic phase was washed with water and saturated sodium chloride solution, dried over sodium sulfate, filtered and concentrated to small volume under vacuum. The crude product was used in the next stage with no further purification. Yield: 90%

후처리

  1. stirringThe mixture was stirred for 16 h at 25° C
  2. customThe solvent was removed under vacuum
  3. dissolutionthe residue dissolved in water
  4. washwashed with diethyl ether
  5. extractionextracted with ethyl acetate
  6. washThis organic phase was washed with water and saturated sodium chloride solution
  7. dry with materialdried over sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated to small volume under vacuum
  10. customThe crude product was used in the next stage with no further purification

출처 및 근거

ORD 기록
ord-327166f8f0304d60b99def0c2983061b
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08278319B2

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