Thiocyanate → 2-(3,4-Dichlorophenyl)-1-hydrazinecarbothioamide

HRID 1665203

Reaction equation

HRID 1665203 reaction equation
[Cl:1][C:2]1[CH:3]=[C:4]([NH:9][NH2:10])[CH:5]=[CH:6][C:7]=1[Cl:8].[S-:11][C:12]#[N:13].[K]>O>[Cl:1][C:2]1[CH:3]=[C:4]([NH:9][NH:10][C:12]([NH2:13])=[S:11])[CH:5]=[CH:6][C:7]=1[Cl:8]

Participants

5

Reactant 3

HCID 9322ThiocyanateHCID 83161(3,4-Dichlorophenyl)hydrazineHCID 5462222Potassium

Product 1

HCID 37596382-(3,4-Dichlorophenyl)-1-hydrazinecarbothioamideYield 95%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

A mixture of 3,4-dichlorophenylhydrazine (18.8 mmol) and thiocyanate of potassium (55.7 mmol) was dissolved in water (1 L) and heated for 17 hours. After cooling the product the solid was filtered and dried in vacuo to give 3,4-dichlorophenylthiosemicarbazide (4.20 g, yield=95%). H1NMR (300 MHz, DMSO, 25° C.) δ: 9.37 (s, 1H); 8.30 (s, 1H); 7.84 (s, 1H); 7.60 (s, 1H); 7.40 (d, J=8.7 Hz, 1H); 6.37 (d, J=2.52 Hz. 1H); 6.60 (dd, J=8.67 Hz, J=2.5 Hz. 1H) ppm. EM (ES+) m/z=236 (100%) [M+H]+.

Workup

  1. temperatureheated for 17 hours
  2. temperatureAfter cooling the product the solid
  3. filtrationwas filtered
  4. customdried in vacuo

Sources & evidence

ORD record
ord-744fab7376ab41578e64f65c2de4503b
Source dataset
uspto-grants-2011_10
Patent number
US08039497B2

Linked notes

Loading…