Sodium Hydroxide → HCID 57436798、化合物

HRID 45987ノート

反応式

HRID 45987 の反応式
[F:1][C:2]([F:25])([F:24])[C:3]1[CH:4]=[C:5]([S:9]([N:12]2[CH2:17][CH2:16][CH2:15][CH2:14][CH:13]2[CH2:18][C:19]([O:21]CC)=[O:20])(=[O:11])=[O:10])[CH:6]=[CH:7][CH:8]=1.[OH-].[Na+]>CO.O1CCOCC1>[F:25][C:2]([F:1])([F:24])[C:3]1[CH:4]=[C:5]([S:9]([N:12]2[CH2:17][CH2:16][CH2:15][CH2:14][CH:13]2[CH2:18][C:19]([OH:21])=[O:20])(=[O:11])=[O:10])[CH:6]=[CH:7][CH:8]=1

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 57819731HCID 57819731、化合物

生成物 1

HCID 57436798HCID 57436798、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回HCID 312751,4-Dioxane溶媒

実験手順

The ethyl 2-(1-(3-(trifluoromethyl)phenylsulfonyl)piperidin-2-yl)acetate (10.45 g, 27.5 mmol) was dissolved in a mixture of methanol (150 ml), dioxane (40 ml) and aqueous NaOH solution (4 M, 41.3 ml, 165.2 mmol, 6 eq.) and the solution was stirred overnight When the reaction had ended (TLC control, MC/methanol 95:5), the solution was concentrated. The crude product was taken up in ethyl acetate (600 ml) and the mixture was . . . with KHSO4 solution (0.5 M, 600 ml). The aqueous phase was extracted once more with ethyl acetate (100 ml) and the combined organic phases were washed with sat. NaCl solution (500 ml), dried over Na2SO4 and concentrated. Yield: 9.4 g, 97%.

後処理

  1. concentrationthe solution was concentrated
  2. extractionThe aqueous phase was extracted once more with ethyl acetate (100 ml)
  3. washthe combined organic phases were washed with sat. NaCl solution (500 ml)
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-e68a6fb3c19b4a778a2232070437c467
出典データセット
uspto-grants-2013_09
特許番号
US08541573B2

反応ノート

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