Water → HCID 12268076、化合物

HRID 585553ノート

反応式

HRID 585553 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 product MS (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 product MS (ESI+) for C9H14O3 m/z 171.2 (M+H)+

出典と根拠

ORDレコード
ord-4b1e42173ce342a1ad81e1f437b3a2f7
出典データセット
uspto-grants-2005_08
特許番号
US06933304B2

反応ノート

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