Ammonium Chloride → HCID 178469800, 화합물

HRID 1913516노트

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HRID 1913516 반응식
C[N:2]([CH3:12])[CH:3]=[C:4]([N+:10]#[C-:11])[C:5]([O:7][CH2:8][CH3:9])=[O:6].[Cl-].[NH4+].[CH3:15][C@H:16]1[CH2:21][CH2:20][C@H](N)[CH2:18][CH2:17]1>>[CH3:15][C@H:16]1[CH2:21][CH2:20][C@H:12]([N:2]2[CH:3]=[C:4]([C:5]([O:7][CH2:8][CH3:9])=[O:6])[N:10]=[CH:11]2)[CH2:18][CH2:17]1

참가 물질

4

반응물 3

HCID 25517Ammonium ChlorideHCID 54355309Ethyl 3-(dimethylamino)-2-isocyanoacrylateHCID 178461305HCID 178461305, 화합물

생성물 1

HCID 178469800HCID 178469800, 화합물수율 89%

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온도
70 °C

실험 절차

Ethyl 3-(dimethylamino)-2-isocyanoacrylate (Liebigs Annalen der Chemie, 1979, p. 1444) (1.52 g) was dissolved in trans-4-methylcyclohexylamine (3.07 g), and the solution was stirred at 70° C. for 4 hours. To the reaction solution, saturated aqueous ammonium chloride was added, and organic matter was extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and filtered, and the solvent was distilled off under reduced pressure to obtain a crude product. This crude product was purified by silica gel column chromatography (eluting solvent: hexane/ethyl acetate=2/1-1/2) to obtain the title compound (1.90 g).

후처리

  1. extractionorganic matter was extracted with ethyl acetate
  2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  3. filtrationfiltered
  4. distillationthe solvent was distilled off under reduced pressure
  5. customto obtain a crude product
  6. customThis crude product was purified by silica gel column chromatography (eluting solvent: hexane/ethyl acetate=2/1-1/2)

출처 및 근거

ORD 기록
ord-249359ebf551447a8c1e3a5f833bad3e
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08609710B2

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