Ethyl bromopyruvate → HCID 18408534, 화합물

HRID 992984노트

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HRID 992984 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:9]=[C:10]([O:14][CH3:15])[C:11]=1[O:12][CH3:13])[C:6](=[S:8])[NH2:7].Br[CH2:17][C:18](=O)[C:19]([O:21][CH2:22][CH3:23])=[O:20]>C(O)C>[CH3:15][O:14][C:10]1[CH:9]=[C:5]([C:6]2[S:8][CH:17]=[C:18]([C:19]([O:21][CH2:22][CH3:23])=[O:20])[N:7]=2)[CH:4]=[C:3]([O:2][CH3:1])[C:11]=1[O:12][CH3:13]

참가 물질

4

반응물 2

HCID 66144Ethyl bromopyruvateHCID 3033195Benzamide, thio-3,4,5-trimethoxy-

생성물 1

HCID 18408534HCID 18408534, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
80 °C

실험 절차

3,4,5-Trimethoxybenzothioamide (2.5 g) and 90% ethyl bromopyruvate (2.62 g) were added to ethanol (20 mL), and the mixture was stirred at 80° C. for 1 hour. The reaction mixture was concentrated under reduced pressure, and the residue was diluted with ethyl acetate, washed with a saturated aqueous solution of sodium hydrogencarbonate, water and saturated brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was then purified by column chromatography on silica gel (hexane:ethyl acetate=1:1) and further recrystallized from ethyl acetate-hexane to obtain the title compound.

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. additionthe residue was diluted with ethyl acetate
  3. washwashed with a saturated aqueous solution of sodium hydrogencarbonate, water and saturated brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was then purified by column chromatography on silica gel (hexane:ethyl acetate=1:1)
  7. customfurther recrystallized from ethyl acetate-hexane

출처 및 근거

ORD 기록
ord-90fdfa3d5b914add8cb01dc678b44b18
출처 데이터셋
uspto-grants-2002_10
특허 번호
US06472386B1

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