Dimethyl Sulfate → Vincamine methylsulfate

HRID 1112367ノート

反応式

HRID 1112367 の反応式
[CH3:1][CH2:2][C@:3]12[CH2:19][C@:18]([OH:24])([C:20]([O:22][CH3:23])=[O:21])[N:17]3[C:9]4=[C:10]([CH2:25][CH2:26][N:7]([C@@H:8]14)[CH2:6][CH2:5][CH2:4]2)[C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][C:16]=13.[CH3:27][O:28][S:29]([O:32]C)(=[O:31])=[O:30]>CC(C)=O>[CH3:1][CH2:2][C@:3]12[CH2:19][C@:18]([OH:24])([C:20]([O:22][CH3:23])=[O:21])[N:17]3[C:9]4=[C:10]([CH2:25][CH2:26][N:7]([C@@H:8]14)[CH2:6][CH2:5][CH2:4]2)[C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][C:16]=13.[CH3:27][O:28][S:29]([O-:32])(=[O:31])=[O:30]

参加物

4

反応物 2

HCID 6497Dimethyl SulfateHCID 15376Vincamine

生成物 1

HCID 86736090Vincamine methylsulfate

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

7.08 g (2.10-2 moles) of vincamine are dissolved in 900 mls of boiling anhydrous acetone. Under stirring, 1.8 mls of dimethylsulfate are added and the resulting mixture is maintained under boiling for 6 hours. The mixture is concentrated to 400 mls and maintained on standing for a night. The mixture is filtered, washed onto the filter with ether and dried in a vacuum furnace at 50° C. There are obtained 7 g of a product having melting point of 191° C., soluble in water and alcohol.

後処理

  1. temperaturethe resulting mixture is maintained
  2. concentrationThe mixture is concentrated to 400 mls
  3. temperaturemaintained
  4. waiton standing for a night
  5. filtrationThe mixture is filtered
  6. washwashed onto the
  7. filtrationfilter with ether
  8. customdried in a vacuum furnace at 50° C

出典と根拠

ORDレコード
ord-9d3c0aeb99d14b63b3e3160bd9e958e9
出典データセット
uspto-grants-1978_10
特許番号
US04122179

反応ノート

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