Isovincamine → Apovincamine

HRID 1414344

反応式

HRID 1414344 の反応式
[CH3:1][CH2:2][C:3]12[CH2:21][C:20](O)([C:22]([O:24][CH3:25])=[O:23])[N:19]3[C:9]4=[C:10]([C:13]5[C:18]3=[CH:17][CH:16]=[CH:15][CH:14]=5)[CH2:11][CH2:12][N:7]([CH:8]14)[CH2:6][CH2:5][CH2:4]2>C(O)=O>[CH3:1][CH2:2][C@:3]12[CH:21]=[C:20]([C:22]([O:24][CH3:25])=[O:23])[N:19]3[C:9]4=[C:10]([CH2:11][CH2:12][N:7]([C@@H:8]14)[CH2:6][CH2:5][CH2:4]2)[C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][C:18]=13

参加物

3

反応物 1

HCID 5668Isovincamine

生成物 1

HCID 71204Apovincamine収率 80.3%

試薬・触媒・溶媒 1

HCID 284Formic Acid溶媒

実験手順

A solution of 3.54 g (0.01 mol) of 16-epivincamine in 50 ml of formic acid is heated under reflux for 10 hours, under nitrogen. The formic acid is evaporated on a water bath in vacuo, the residue is dissolved in methylene chloride, and the latter solution is washed with a saturated solution of sodium bicarbonate and with water. The solution is dried over sodium sulphate and filtered, and the methylene chloride is evaporated from the filtrate. 2.7g (yield = 80%) of apovincamine are thus collected.

後処理

  1. temperatureunder reflux for 10 hours, under nitrogen
  2. customThe formic acid is evaporated on a water bath in vacuo
  3. dissolutionthe residue is dissolved in methylene chloride
  4. washthe latter solution is washed with a saturated solution of sodium bicarbonate and with water
  5. dry with materialThe solution is dried over sodium sulphate
  6. filtrationfiltered
  7. customthe methylene chloride is evaporated from the filtrate

出典と根拠

ORDレコード
ord-9c7eaee7879a416981dc934ca6fde6c3
出典データセット
uspto-grants-1977_01
特許番号
US04001251

関連ノート

読み込み中…