Water → HCID 12268076, 화합물

HRID 1243518노트

반응식

HRID 1243518 반응식
[CH3:1][C:2]1([CH2:14][CH2:15][CH3:16])[CH:7](C#N)[C:6](=[O:10])N[C:4](=[O:11])[CH:3]1C#N.[OH2:17]>S(=O)(=O)(O)O>[CH3:1][C:2]1([CH2:14][CH2:15][CH3:16])[CH2:3][C:4](=[O:11])[O:17][C:6](=[O:10])[CH2:7]1

참가 물질

4

반응물 2

HCID 962WaterHCID 9585664635-91-2

생성물 1

HCID 12268076HCID 12268076, 화합물

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

반응 조건

온도
130 °C

실험 절차

Following the procedure of Vogel, A. I.; J. Chem. Soc., 1934; 1758–1765: 4-Methyl-2,6-dioxo-4-propyl-piperidine-3,5-dicarbonitrile was dissolved in 50 mL of sulfuric acid and stirred for 16 hrs. Water (50 mL) was added and the solution was refluxed for 18 hrs. Upon cooling, the crystals were collected. The crystals were suspended in 10 mL of acetic anhydride. The suspension was heated to 130° C. and stirred for 16 hrs. The solvent was removed under reduced pressure. The residue was partitioned between saturated aqueous sodium bicarbonate and diethyl ether. The ether fraction was treated with anhydrous magnesium sulfate and concentrated under reduced pressure to give the productMS (ESI+) for C9H14O3 m/z 171.2 (M+H)+.

후처리

  1. temperaturethe solution was refluxed for 18 hrs
  2. temperatureUpon cooling
  3. customthe crystals were collected
  4. stirringstirred for 16 hrs
  5. customThe solvent was removed under reduced pressure
  6. customThe residue was partitioned between saturated aqueous sodium bicarbonate and diethyl ether
  7. additionThe ether fraction was treated with anhydrous magnesium sulfate
  8. concentrationconcentrated under reduced pressure
  9. customto give the productMS (ESI+) for C9H14O3 m/z 171.2 (M+H)+

출처 및 근거

ORD 기록
ord-eb8dc95f2d5d4803b436be79ccba9609
출처 데이터셋
uspto-grants-2006_10
특허 번호
US07119098B2

반응 노트

불러오는 중…