2-Propenoic acid, 3-(tetrahydro-2H-thiopyran-4-yl)-, ethyl ester → HCID 20143673, compound

HRID 980617Notes

Reaction equation

HRID 980617 reaction equation
[S:1]1[CH2:6][CH2:5][CH:4]([CH:7]=[CH:8][C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH2:3][CH2:2]1>C(O)C.[C].[Pd]>[S:1]1[CH2:6][CH2:5][CH:4]([CH2:7][CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH2:3][CH2:2]1

Participants

4

Conditions

Temperature
50 °C

Procedure

In 150 ml of ethanol is dissolved 10 g of ethyl 3-(4-thianyl)acrylate, and a catalytic reduction reaction is carried out at ordinary temperature and at atmospheric pressure using 9 g of 10% palladium-carbon (50% in water) as a catalyst. The reaction mixture is stirred at room temperature for 20 minutes and at 50° C. for 8 hours, and the catalyst is removed by filtration. Nine (9) g of 10% palladium-carbon (50% in water) is added anew to the filtrate, followed by stirring at 50° C. for one day. The catalyst is removed by filtration, and the filtrate is concentrated under reduced pressure to give 9.1 g of ethyl 3-(4-thianyl)propionate as an oily material.

Workup

  1. customa catalytic reduction reaction
  2. customthe catalyst is removed by filtration
  3. additionNine (9) g of 10% palladium-carbon (50% in water) is added anew to the filtrate
  4. stirringby stirring at 50° C. for one day
  5. customThe catalyst is removed by filtration
  6. concentrationthe filtrate is concentrated under reduced pressure

Sources & evidence

ORD record
ord-55616787f6f74eb4ae1bda109fc5bba8
Source dataset
uspto-grants-1987_01
Patent number
US04638000

Reaction notes

Loading…