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Acetic Anhydride → HCID 14881376, 화합물

HRID 1608340
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HRID 1608340 반응식
[C:1]([O:4][C:5](=[O:7])[CH3:6])(=O)[CH3:2].OCC[N:11]1[C:16]([CH3:17])=[C:15]([CH3:18])[N:14]=[C:13]([CH3:19])[C:12]1=[O:20]>N1C=CC=CC=1>[C:5]([O:4][CH2:1][CH2:2][N:11]1[C:16]([CH3:17])=[C:15]([CH3:18])[N:14]=[C:13]([CH3:19])[C:12]1=[O:20])(=[O:7])[CH3:6]
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참가 물질

4

반응물 2

HCID 7918Acetic AnhydrideHCID 147735301-(2-Hydroxyethyl)-3,5,6-trimethylpyrazin-2-one

생성물 1

HCID 14881376HCID 14881376, 화합물수율 51.8%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

Acetic anhydride (2 ml) was added under ice-cooling to compound 026 (0.91 g, 5 mM) dissolved in pyridine (10 ml), and stirred at room temperature for 1.5 hours. The reaction mixture was concentrated in vacuo and dilute aqueous K2CO3 was added thereto, the resultant mixture being extracted three times with chloroform. The extract was dried with anhydrous magnesium sulfate and concentrated in vacuo. The residue was charged on a column of silica-gel (Florisil, 60 g) packed with benzene and eluted with benzene-ethyl acetate (5:1) to obtain compound 061 (0.58 g, yield: 51.8%).

후처리

  1. concentrationThe reaction mixture was concentrated in vacuo and dilute aqueous K2CO3
  2. additionwas added
  3. extractionthe resultant mixture being extracted three times with chloroform
  4. dry with materialThe extract was dried with anhydrous magnesium sulfate
  5. concentrationconcentrated in vacuo
  6. additionThe residue was charged on a column of silica-gel (Florisil, 60 g)
  7. washeluted with benzene-ethyl acetate (5:1)

출처 및 근거

ORD 기록
ord-0e900a35f7e4440a83d0739fbf32b63f
출처 데이터셋
uspto-grants-1989_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04870176

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