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

HRID 536709노트

반응식

HRID 536709 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

실험 절차

A mixture of Example 27B (13.5 g, 85 mmol) and 4,4-dimethyl-3-oxopentanenitrile (11.69 g, 93 mmol) in ethanol (50 mL) was refluxed at 90° C. for 6 hours. The mixture was concentrated under reduced pressure and ethyl acetate (20 mL) added to the residue. The white solid precipitate was filtered, washed with ether and dried to yield 17.5 g (90%) of title compound as a white solid. 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. concentrationThe mixture was concentrated under reduced pressure and ethyl acetate (20 mL)
  2. additionadded to the residue
  3. filtrationThe white solid precipitate was filtered
  4. washwashed with ether
  5. customdried

출처 및 근거

ORD 기록
ord-d470002338e24e90b2fc5c230bad2bfc
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08859596B2

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