Water → HCID 12268076、化合物

HRID 1243518ノート

反応式

HRID 1243518 の反応式
[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

参加物

4

反応物 2

HCID 962WaterHCID 9585664635-91-2

生成物 1

HCID 12268076HCID 12268076、化合物

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

反応条件

温度
130 °C

実験手順

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)+.

後処理

  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)+

出典と根拠

ORDレコード
ord-eb8dc95f2d5d4803b436be79ccba9609
出典データセット
uspto-grants-2006_10
特許番号
US07119098B2

反応ノート

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