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Pyridine → HCID 86667488, 화합물

HRID 1847123
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HRID 1847123 반응식
[CH3:1][CH:2]([CH2:4][CH2:5][CH2:6][C@@H:7]([C@@H:9]1[C@:26]2([CH3:27])[C@H:12]([C:13]3[O:14][C:15](=[O:29])[CH:16]4[C@:21]([C:23]=3[CH2:24][CH2:25]2)([CH3:22])[CH2:20][CH2:19][C:18](=O)[CH2:17]4)[CH2:11][CH2:10]1)[CH3:8])[CH3:3].Cl.[CH3:31][O:32][NH2:33].N1C=CC=CC=1.[Cl-].[NH4+]>C(O)C>[CH3:31][O:32][N:33]=[C:18]1[CH2:19][CH2:20][C@@:21]2([CH3:22])[CH:16]([C:15](=[O:29])[O:14][C:13]3[C@H:12]4[C@:26]([CH3:27])([CH2:25][CH2:24][C:23]=32)[C@@H:9]([C@@H:7]([CH3:8])[CH2:6][CH2:5][CH2:4][CH:2]([CH3:3])[CH3:1])[CH2:10][CH2:11]4)[CH2:17]1
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참가 물질

6

반응물 4

HCID 1049PyridineHCID 25517Ammonium ChlorideHCID 521874O-Methylhydroxylamine hydrochlorideHCID 67609998HCID 67609998, 화합물

생성물 1

HCID 86667488HCID 86667488, 화합물수율 93%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Compound 1 (40 mg, 0.10 mmol) obtained in Example 1 was dissolved in ethanol (5 mL), and O-methylhydroxyamine hydrochloride (25 mg, 0.30 mmol) and pyridine (0.024 mL, 0.03 mmol) were added thereto, followed by stirring at room temperature for 3 hours. A saturated aqueous ammonium chloride solution was added to the reaction mixture, followed by extraction with ethyl acetate twice. The organic layer was dried over anhydrous sodium sulfate, and concentrated under reduced pressure to yield a residue. The residue was purified by preparative thin layer chromatography to obtain the title compound (39 mg, 93%) as an E/Z mixture.

후처리

  1. extractionfollowed by extraction with ethyl acetate twice
  2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customto yield a residue
  5. customThe residue was purified by preparative thin layer chromatography

출처 및 근거

ORD 기록
ord-6b7e61fe82694da6a3fd49512d290b6c
출처 데이터셋
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08952003B2

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