2,4,6-Trimethylbenzoyl chloride → HCID 14556374, compound

HRID 1533856Notes

Reaction equation

HRID 1533856 reaction equation
[NH2:1][NH:2][C:3]([NH2:5])=[S:4].[CH3:6][C:7]1[CH:15]=[C:14]([CH3:16])[CH:13]=[C:12]([CH3:17])[C:8]=1[C:9](Cl)=[O:10]>CN(C)C=O.N1C=CC=CC=1>[CH3:6][C:7]1[CH:15]=[C:14]([CH3:16])[CH:13]=[C:12]([CH3:17])[C:8]=1[C:9]([NH:1][NH:2][C:3]([NH2:5])=[S:4])=[O:10]

Participants

5

Reactant 2

HCID 970382,4,6-Trimethylbenzoyl chlorideHCID 2723789Thiosemicarbazide

Product 1

HCID 14556374HCID 14556374, compound

Reagents, catalysts & solvents 2

HCID 1049PyridineSolventHCID 6228DimethylformamideSolvent

Conditions

Temperature
80 °C

Procedure

37.25 g of thiosemicarbazide was dissolved in 400 ml dimethylformamide and 32.05 g of pyridine, after which 74 g of 2,4,6-trimethylbenzoyl chloride was added at 0° C. in 20 minutes. The reaction mixture was heated at 80° C. for 2 hours and then concentrated to three-quarters in vacuo and the remaining mixture was poured into 1500 ml of cold water. The resulting white precipitate was filtered, washed in water and dried.

Workup

  1. concentrationconcentrated to three-quarters in vacuo
  2. additionthe remaining mixture was poured into 1500 ml of cold water
  3. filtrationThe resulting white precipitate was filtered
  4. washwashed in water
  5. customdried

Sources & evidence

ORD record
ord-ffd2d91c1e1646cc92f82e41644a3510
Source dataset
uspto-grants-1992_02
Patent number
US05086053

Reaction notes

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