Water → HCID 23667320, compound

HRID 436390Notes

Reaction equation

HRID 436390 reaction equation
[OH-].[K+:2].O.[CH3:4][N:5]1[CH2:10][CH2:9][NH:8][CH2:7][CH2:6]1.[C:11](=[S:13])=[S:12]>C1(C)C=CC=CC=1>[C:11](=[S:13])([S-:12])[NH2:5].[CH3:4][N:5]1[CH2:10][CH2:9][NH:8][CH2:7][CH2:6]1.[K+:2]

Participants

6

Reactant 4

HCID 962WaterHCID 6348Carbon Disulfide2×HCID 14797Potassium HydroxideHCID 531671-Methylpiperazine

Product 1

HCID 23667320HCID 23667320, compound

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Conditions

Temperature
20 °C

Procedure

To a 3-necked round bottom flask equipped with a mechanical stirrer, addition funnel and reflux condenser was added 3.12 grams of 90% potassium hydroxide, 100 ml. of water and 60 grams of N-methylpiperazine. The solution was cooled to 20° C with an ice bath and thereafter 38 grams of carbon disulfide was added drop-wise. When the addition of carbon disulfide had been completed, 100 ml. toluene was added and a Dean-Stark trap placed on the flask. The water was azeotroped off, followed by distillation of toluene. The solid salt was then dissolved in an equal amount of diethylene glycol to give a 50% solution of potassium N-methylpiperazine dithiocarbamate.

Workup

  1. customTo a 3-necked round bottom flask equipped with a mechanical stirrer, addition funnel
  2. temperaturereflux condenser
  3. customThe water was azeotroped off
  4. distillationfollowed by distillation of toluene
  5. dissolutionThe solid salt was then dissolved in an equal amount of diethylene glycol

Sources & evidence

ORD record
ord-350924de7c9040b5a12ed60385b574da
Source dataset
uspto-grants-1977_02
Patent number
US04009130

Reaction notes

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