Hydrochloric Acid → HCID 178505461, compound

HRID 555814Notes

Reaction equation

HRID 555814 reaction equation
[F:1][C:2]1[CH:3]=[C:4](N)[C:5]([NH2:8])=[CH:6][CH:7]=1.[C:10]([S-:15])(=[S:14])OCC.[K+].O.Cl>CN(C=O)C>[F:1][C:2]1[CH:7]=[CH:6][C:5]2[N:8]=[C:10]([SH:15])[S:14][C:4]=2[CH:3]=1

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 1645844-Fluorobenzene-1,2-diamineHCID 2735045Potassium ethylxanthate

Product 1

HCID 178505461HCID 178505461, compound

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Conditions

Temperature
95 °C

Procedure

4-Fluorobenzene-1,2-diamine (10.0 g, 0.077 mol) and potassium O-ethyl carbonodithioate (37.1 g, 0.234 mol) were dissolved in dry DMF (150 mL) under nitrogen and heated to 95° C. for 12 h. The reaction was cooled to RT and 200 mL water was added followed by addition of 5N HCl to get precipitates. After stirring for 1 h, the precipitates were collected by filtration, washed with water and dried under vacuum for 2 h. The crude compound was then washed with chloroform and dried to give 6-fluorobenzo[d]thiazole-2-thiol as yellow solid.

Workup

  1. temperatureThe reaction was cooled to RT
  2. customto get
  3. customprecipitates
  4. filtrationthe precipitates were collected by filtration
  5. washwashed with water
  6. customdried under vacuum for 2 h
  7. washThe crude compound was then washed with chloroform
  8. customdried

Sources & evidence

ORD record
ord-13c7f6e11af743ab90fc114837dfcdf6
Source dataset
uspto-grants-2011_11
Patent number
US08053438B2

Reaction notes

Loading…