Barium hydroxide → HCID 39733728、化合物

HRID 1808335ノート

反応式

HRID 1808335 の反応式
[OH-:1].[Ba+2].[OH-:3].O1CCN([C:10](=S)[CH2:11][C:12]2[CH:21]=[C:20]3[C:15]([CH2:16][CH2:17][CH2:18][NH:19]3)=[CH:14][CH:13]=2)CC1>C(O)C>[NH:19]1[C:20]2[C:15](=[CH:14][CH:13]=[C:12]([CH2:11][C:10]([OH:3])=[O:1])[CH:21]=2)[CH2:16][CH2:17][CH2:18]1

参加物

4

反応物 2

HCID 6093286Barium hydroxideHCID 86645316HCID 86645316、化合物

生成物 1

HCID 39733728HCID 39733728、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
80 °C

実験手順

110 ml of a 20% barium hydroxide solution were added dropwise to a solution of 1-morpholino-2-(1,2,3,4-tetrahydroquinolin-7-yl)-ethanethione (11 g; 1 equiv.) in 55 ml of ethanol, and the resulting reaction mixture was heated for 10 hours at reflux. When the conversion was complete, the solvent was removed under reduced pressure and the residue was taken up in 100 ml of water and heated to 80° C. The reaction mixture was then neutralised carefully with dry ice, filtered over Celite and concentrated under reduced pressure. The resulting crude product (14 g) was used in the next stage without further purification.

後処理

  1. customthe resulting reaction mixture
  2. temperaturewas heated for 10 hours
  3. temperatureat reflux
  4. customthe solvent was removed under reduced pressure
  5. filtrationfiltered over Celite
  6. concentrationconcentrated under reduced pressure
  7. customThe resulting crude product (14 g) was used in the next stage without further purification

出典と根拠

ORDレコード
ord-b969773ccd7b4931822e4bb147008098
出典データセット
uspto-grants-2013_01
特許番号
US08357717B2

反応ノート

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