Lithium Hydroxide → HCID 57436798、化合物

HRID 2059897ノート

反応式

HRID 2059897 の反応式
[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

参加物

5

反応物 2

HCID 3939Lithium HydroxideHCID 58711709HCID 58711709、化合物

生成物 1

HCID 57436798HCID 57436798、化合物収率 90%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

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%

後処理

  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

出典と根拠

ORDレコード
ord-327166f8f0304d60b99def0c2983061b
出典データセット
uspto-grants-2012_10
特許番号
US08278319B2

反応ノート

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