2,2',4'-Trichloroacetophenone → HCID 178482494, compound

HRID 1105562Notes

Reaction equation

HRID 1105562 reaction equation
[Cl:1][C:2]1[CH:11]=[C:10]([Cl:12])[CH:9]=[CH:8][C:3]=1[C:4](=O)[CH2:5]Cl.[CH3:13][NH:14][C:15](=[S:18])[NH:16][NH2:17]>CO>[ClH:1].[Cl:1][C:2]1[CH:11]=[C:10]([Cl:12])[CH:9]=[CH:8][C:3]=1[C:4]1[CH2:5][S:18][C:15]([NH:14][CH3:13])=[N:16][N:17]=1

Participants

4

Reactant 2

HCID 202502,2',4'-TrichloroacetophenoneHCID 2723853N-Methylhydrazinecarbothioamide

Product 1

HCID 178482494HCID 178482494, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

11.17 g of 2,4-dichlorophenacyl chloride and 5.755 g of 4-methyl-thiosemicarbazide are reacted in 200 ml of methanol using the procedure of Example 2. The initial crystallization is made from methanol/ethyl acetate. The solid is then recrystallized from methanol/ethyl acetate and dried at 65° C. under high vacuum to produce 5-(2,4-dichlorophenyl)-N-methyl-6H-1,3,4-thiadiazin-2-amine monohydrochloride. m.p. 195° C.

Workup

  1. customThe initial crystallization
  2. customThe solid is then recrystallized from methanol/ethyl acetate
  3. customdried at 65° C. under high vacuum

Sources & evidence

ORD record
ord-e143c5f77cc0436fb3f42c09f6c8e928
Source dataset
uspto-grants-1982_01
Patent number
US04309426

Reaction notes

Loading…