Potassium Carbonate → HCID 13487836, compound

HRID 1711171Notes

Reaction equation

HRID 1711171 reaction equation
[C:1]([N:4](C(=O)C)[C:5](=[N:8][CH3:9])[S:6][CH3:7])(=[O:3])[CH3:2].C([O-])([O-])=O.[K+].[K+]>CO>[C:1]([NH:4][C:5](=[N:8][CH3:9])[S:6][CH3:7])(=[O:3])[CH3:2]

Participants

4

Reactant 2

HCID 11430Potassium CarbonateHCID 86629530HCID 86629530, compound

Product 1

HCID 13487836HCID 13487836, compoundYield 85.1%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

To a solution of 1,1-diacetyl-2,3-dimethyl-isothiourea (0.17 g, 0.90 mmol) in MeOH (10 ml) was added K2CO3 (250 mg, 1.81 mmol) and the reaction stirred at room temperature for 1.5 h. The mixture was concentrated, diluted with CH2Cl2 (25 ml) and water (20 ml) and the aqueous layer was extracted with CH2Cl2 (2×10 ml), dried (Na2SO4) and concentrated to afford 1-acetyl-2,3-dimethyl-isothiourea (112 mg, 85%) as a white solid. 1H NMR (CDCl3) δ 2.10 (s, 3H), 2.43 (s, 3H), 2.93 (s, 3H).

Workup

  1. concentrationThe mixture was concentrated
  2. additiondiluted with CH2Cl2 (25 ml) and water (20 ml)
  3. extractionthe aqueous layer was extracted with CH2Cl2 (2×10 ml)
  4. dry with materialdried (Na2SO4)
  5. concentrationconcentrated

Sources & evidence

ORD record
ord-52d691c6e3d84101aefb14caabd6a3cf
Source dataset
uspto-grants-2010_09
Patent number
US07790747B2

Reaction notes

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