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

HRID 883021노트

반응식

HRID 883021 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 1B (13.5 g, 85 mmol) and 4,4-dimethyl-3-oxopentanenitrile (11.7 g, 93 mmol) in ethanol (100 mL) was heated at reflux 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 precipitate was filtered, washed with ether, and dried to yield 17.5 g (90%) of title compound. 1H NMR (300 MHz, DMSO-d6) δ ppm 0.42-0.54 (m, 4 H), 1.16-1.27 (m, 1 H), 1.28 (s, 9 H), 4.38 (d, J=7.12 Hz, 2 H), 4.80 (br, 2 H), 5.53 (s, 1 H), 15.5 (br, 1 H); MS (DCI) m/z 194 [M+H]+.

후처리

  1. temperatureat reflux for 6 hours
  2. concentrationconcentrated under reduced pressure
  3. additionThe residue was diluted with ethyl acetate (20 mL)
  4. filtrationThe resulting white precipitate was filtered
  5. washwashed with ether
  6. customdried

출처 및 근거

ORD 기록
ord-f4f76006a7f142d0a4fc517c89a5c429
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08236822B2

반응 노트

불러오는 중…