Pentanenitrile, 4,4-dimethyl-3-oxo- → HCID 66644209, 화합물

HRID 2064499노트

반응식

HRID 2064499 반응식
[ClH:1].Cl.[CH:3]1([CH2:6][NH:7][NH2:8])[CH2:5][CH2:4]1.[CH3:9][C:10]([CH3:17])([CH3:16])[C:11](=O)[CH2:12][C:13]#[N:14]>C(O)C>[ClH:1].[C:10]([C:11]1[CH:12]=[C:13]([NH2:14])[N:7]([CH2:6][CH:3]2[CH2:5][CH2:4]2)[N:8]=1)([CH3:17])([CH3:16])[CH3:9]

참가 물질

4

반응물 2

HCID 108871Pentanenitrile, 4,4-dimethyl-3-oxo-HCID 43810474(Cyclopropylmethyl)hydrazine--hydrogen chloride (1/2)

생성물 1

HCID 66644209HCID 66644209, 화합물수율 90%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
90 °C

실험 절차

A mixture of Example 9B (13.5 g, 85 mmol) and 4,4-dimethyl-3-oxopentanenitrile (11.69 g, 93 mmol) in ethanol (100 mL) was heated at reflux (oil bath temperature of 90° C.) for 6 hours. The mixture was cooled to room temperature, and concentrated under reduced pressure. The residue was diluted with ethyl acetate (20 mL). The resulting white solid was collected by filtration (Et2O wash) and dried to provide 17.5 g (90%) of title compound. 1H NMR (300 MHz, DMSO-d6) δ ppm 0.42-0.54 (m, 4H), 1.16-1.27 (m, 1H), 1.28 (s, 9H), 4.02 (d, J=7.12 Hz, 2H), 5.53 (s, 1H), 6.91 (s, 2H), 14.05 (s, 1H); MS (DCI) m/z 294 [M+H]+.

후처리

  1. temperatureThe mixture was cooled to room temperature
  2. concentrationconcentrated under reduced pressure
  3. additionThe residue was diluted with ethyl acetate (20 mL)
  4. filtrationThe resulting white solid was collected by filtration (Et2O wash)
  5. customdried

출처 및 근거

ORD 기록
ord-58a6c67390c14971bfcd427a2c250346
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08288428B2

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