Cyclopropylacetonitrile → tert-Butyl 4-[cyano(cyclopropyl)methylidene]piperidine-1-carboxylate

HRID 1852457

반응식

HRID 1852457 반응식
O=[C:2]1[CH2:7][CH2:6][N:5]([C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9])[CH2:4][CH2:3]1.[CH:15]1([CH2:18][C:19]#[N:20])[CH2:17][CH2:16]1>C1COCC1>[C:19]([C:18]([CH:15]1[CH2:17][CH2:16]1)=[C:2]1[CH2:7][CH2:6][N:5]([C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9])[CH2:4][CH2:3]1)#[N:20]

참가 물질

4

반응물 2

HCID 643447CyclopropylacetonitrileHCID 735900tert-Butyl 4-oxopiperidine-1-carboxylate

생성물 1

HCID 86729356tert-Butyl 4-[cyano(cyclopropyl)methylidene]piperidine-1-carboxylate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

tert-Butyl 4-oxopiperidine-1-carboxylate (2.0 g, 10 mmol) and cyclopropylacetonitrile (0.97 g, 12 mmol) were dissolved in THF (20 mL), heated to reflux, and allowed to stir for 3 hours. The mixture was then cooled to ambient temperature and concentrated in vacuo. The residue was purified by MPLC on silica gel to afford the title compound as a white solid. LRMS (ESI) calc'd for C15H23N2O2 [M+H]+ 263. Found 263.

후처리

  1. temperatureheated
  2. temperatureto reflux
  3. concentrationconcentrated in vacuo
  4. customThe residue was purified by MPLC on silica gel

출처 및 근거

ORD 기록
ord-ff596dcf29774780af7dedd410c91a22
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08962608B2

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