Hydrochloric Acid → HCID 21186672、化合物

HRID 1384264ノート

反応式

HRID 1384264 の反応式
[CH3:1][C:2]1[N:7]=[C:6]2[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][C:5]2=[CH:4][C:3]=1[C:13]([O:15]CC)=[O:14].Cl>[OH-].[Na+]>[CH3:1][C:2]1[N:7]=[C:6]2[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][C:5]2=[CH:4][C:3]=1[C:13]([OH:15])=[O:14]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 21186750HCID 21186750、化合物

生成物 1

HCID 21186672HCID 21186672、化合物収率 72.7%

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

実験手順

Ethyl 2-methyl-6,7,8,9-tetrahydro-5H-cyclohepta[b]pyridine-3-carboxylate (3.05 g, 13.1 mmol) was suspended in 5% sodium hydroxide aqueous solution (20.0 ml) and heated under reflux for 1 hour. After cooling to room temperature, this was adjusted to pH 4 by adding concentrated hydrochloric acid and extracted with chloroform-methanol (4:1) mixed solvent. The thus obtained organic layer was washed with saturated brine and then dried over anhydrous sodium sulfate. By evaporating the solvent under reduced pressure, the title compound (1.95 g, 72.7%) was obtained as pale brown powder.

後処理

  1. temperatureheated
  2. temperatureunder reflux for 1 hour
  3. extractionextracted with chloroform-methanol (4:1)
  4. additionmixed solvent
  5. washThe thus obtained organic layer was washed with saturated brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. customBy evaporating the solvent under reduced pressure

出典と根拠

ORDレコード
ord-76ceae29ce494296ab4dbf8d8c16e20a
出典データセット
uspto-grants-2001_07
特許番号
US06258829B1

反応ノート

読み込み中…