Sulfuric Acid → HCID 22007848, compound

HRID 253067Notes

Reaction equation

HRID 253067 reaction equation
[CH3:1][C:2]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[Cl:21])([N:6]1[CH2:11][CH2:10][C:9]2[S:12][CH:13]=[CH:14][C:8]=2[CH2:7]1)[C:3]([O-:5])=[O:4].[OH:22][S:23]([OH:26])(=[O:25])=[O:24]>CC(C)=O>[S:23](=[O:24])(=[O:22])([OH:26])[OH:25].[CH3:1][C:2]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[Cl:21])([N:6]1[CH2:11][CH2:10][C:9]2[S:12][CH:13]=[CH:14][C:8]=2[CH2:7]1)[C:3]([OH:5])=[O:4]

Participants

4

Reactant 2

HCID 1118Sulfuric AcidHCID 17769726HCID 17769726, compound

Product 1

HCID 22007848HCID 22007848, compound

Reagents, catalysts & solvents 1

HCID 180AcetoneSolvent

Conditions

Temperature
20 °C

Procedure

2.1 g (+)-Methyl(2-chlorophenyl)-(6,7-dihydro-4H-thieno[3,2-c]pyrid-5-yl)acetate was added 7.6 mL of acetone to obtain a clear solution. To this solution, 0.887 g of H2SO4 (80%) was added slowly and temperature was maintained around 20° C. under nitrogen atmosphere. Later the reaction mixture was cooled up to −20° C. for 2 hrs and then the temperature was brought to room temperature (20° C.). The reaction mixture was stirred at 20-25° C. Precipitate was isolated (600 mg), dried under vacuum at temperature not exceeding 50° C.

Workup

  1. customto obtain a clear solution
  2. temperatureLater the reaction mixture was cooled up to −20° C. for 2 hrs
  3. customwas brought to room temperature
  4. custom(20° C.)
  5. customPrecipitate was isolated (600 mg)
  6. customdried under vacuum at temperature not
  7. customexceeding 50° C.

Sources & evidence

ORD record
ord-11c6d631c07b417a9e804c07435fd238
Source dataset
uspto-grants-2011_01
Patent number
US07872019B2

Reaction notes

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