Pentanenitrile, 4,4-dimethyl-3-oxo- → HCID 63278673, 화합물

HRID 536712노트

반응식

HRID 536712 반응식
Cl.Cl.[F:3][C:4]1[CH:12]=[CH:11][C:7]([CH2:8][NH:9][NH2:10])=[CH:6][CH:5]=1.[CH3:13][C:14]([CH3:21])([CH3:20])[C:15](=O)[CH2:16][C:17]#[N:18]>C(O)C>[C:14]([C:15]1[CH:16]=[C:17]([NH2:18])[N:9]([CH2:8][C:7]2[CH:11]=[CH:12][C:4]([F:3])=[CH:5][CH:6]=2)[N:10]=1)([CH3:21])([CH3:20])[CH3:13]

참가 물질

4

반응물 2

HCID 108871Pentanenitrile, 4,4-dimethyl-3-oxo-HCID 45074965(4-Fluorobenzyl)hydrazine dihydrochloride

생성물 1

HCID 63278673HCID 63278673, 화합물수율 111.8%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
85 °C

실험 절차

To a solution of (4-fluorobenzyl)hydrazine dihydrochloride (1.0 g, 4.7 mmol, Matrix) in ethyl alcohol (2 mL) was added 4,4-dimethyl-3-oxopentanenitrile (0.6 g, 4.7 mmol, Aldrich). After stirring at 85° C. for 2 h, the reaction mixture was cooled, concentrated, diluted with ethyl acetate (10 mL) and washed with saturated NaHCO3 (10 mL). The aqueous layer was extracted with ethyl acetate (2×10 mL). The combined organic extracts were dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure to obtain 1.3 g (99%) of the title compound. MS (ESI+) m/z 248 (M+H)+.

후처리

  1. temperaturethe reaction mixture was cooled
  2. concentrationconcentrated
  3. additiondiluted with ethyl acetate (10 mL)
  4. washwashed with saturated NaHCO3 (10 mL)
  5. extractionThe aqueous layer was extracted with ethyl acetate (2×10 mL)
  6. dry with materialThe combined organic extracts were dried over anhydrous Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-a1eaf6b3cad1416a83c89432f6416c8f
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08859596B2

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