Hydrogen Sulfide → HCID 88518758, compound

HRID 1460611Notes

Reaction equation

HRID 1460611 reaction equation
[C:1]1([CH:7]([Ge:12](Cl)(Cl)Cl)[CH2:8][C:9]([OH:11])=[O:10])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.N1C=CC=CC=1.S>CC(C)=O>[C:1]1([CH:7]([GeH3:12])[CH2:8][C:9]([OH:11])=[O:10])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

Participants

5

Reactant 3

HCID 402Hydrogen SulfideHCID 1049PyridineHCID 13335370HCID 13335370, compound

Product 1

HCID 88518758HCID 88518758, compound

Reagents, catalysts & solvents 1

HCID 180AcetoneSolvent

Procedure

16.4 g (0.05 mol) of 3-phenyl-3-(trichlorogermyl) propionic acid was dissolved in 200 ml of anhydrous acetone. 12.6 g (0.16 mol) of anhydrous pyridine was added to the solution under cooling with an ice bath, followed by stirring. Dry hydrogen sulfide was introduced into the mixture for one hour. The acetone was removed and the residue was dissolved in 50 ml of ethanol. The solution was added to 400 ml of water to precipitate the crystal. The crystal was recrystallized from a mixture of methyl acetate and benzene (1:3) to obtain 12.7 g of crystalline sesquisulfide of 3-phenyl-3-germylpropionic acid. ##STR14##

Workup

  1. temperatureunder cooling with an ice bath
  2. customThe acetone was removed
  3. dissolutionthe residue was dissolved in 50 ml of ethanol
  4. additionThe solution was added to 400 ml of water
  5. customto precipitate the crystal
  6. customThe crystal was recrystallized from a mixture of methyl acetate and benzene (1:3)

Sources & evidence

ORD record
ord-acff000ba2cb4c259a51877f0d8a83f8
Source dataset
uspto-grants-1991_12
Patent number
US05071873

Reaction notes

Loading…