Barium hydroxide → HCID 39733728, compound

HRID 1808335Notes

Reaction equation

HRID 1808335 reaction equation
[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

Participants

4

Reactant 2

HCID 6093286Barium hydroxideHCID 86645316HCID 86645316, compound

Product 1

HCID 39733728HCID 39733728, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Conditions

Temperature
80 °C

Procedure

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.

Workup

  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

Sources & evidence

ORD record
ord-b969773ccd7b4931822e4bb147008098
Source dataset
uspto-grants-2013_01
Patent number
US08357717B2

Reaction notes

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