Sodium Hydroxide → HCID 57436798, 화합물

HRID 45987노트

반응식

HRID 45987 반응식
[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

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 57819731HCID 57819731, 화합물

생성물 1

HCID 57436798HCID 57436798, 화합물

시약·촉매·용매 2

HCID 887Methanol용매2회HCID 312751,4-Dioxane용매

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-e68a6fb3c19b4a778a2232070437c467
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08541573B2

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