Ammonia → Accelerator DM

HRID 637763

Reaction equation

HRID 637763 reaction equation
[SH:1][C:2]1[S:3][C:4]2[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=1.[NH3:11]>C([O-])(=O)C.[Cu+2].C([O-])(=O)C.C(O)(C)C>[CH:8]1[CH:7]=[C:5]2[N:6]=[C:2]([S:1][S:1][C:2]3[S:3][C:4]4[C:5](=[CH:7][CH:8]=[CH:9][CH:10]=4)[N:11]=3)[S:3][C:4]2=[CH:10][CH:9]=1

Participants

5

Reactant 2

HCID 222AmmoniaHCID 178418395HCID 178418395, compound

Product 1

HCID 8447Accelerator DM

Reagents, catalysts & solvents 2

HCID 8895Cupric acetateCatalystHCID 3776IsopropanolSolvent

Conditions

Temperature
70 °C

Procedure

40 g (0.24 mol) of 2-mercaptobenzothiazole (MBT), 4 mg (0.02×10-3 mol) of copper (II) acetate, (Cu(OAc)2. H2O), 4.08 g (0.24 mol) of ammonia, and 120 g of isopropanol are placed in a glass autoclave equipped with a jacket for the circulation of a heating liquid, a thermometer, a pressure measuring device and a stirring device. The reaction mixture is heated to 70° C., stirred vigorously, and placed under an oxygen pressure of 4 bar. Absorption of oxygen is noted immediately and a precipitate, dibenzothiazyl disulfide (MBTS), is formed. After 6.5 hours the reaction is discontinued and the precipitate is filtered off, washed with isopropanol, and dried under a vacuum at 50° C. 37.8 g of a product are obtained in this manner. Upon elementary analysis, IR, NMR and MS, the product formed is found to correspond to dibenzothiazyl disulfide. The purity is found to be 100% upon chromatographic analysis (melting point 178° C.).

Workup

  1. customequipped with a jacket for the circulation of a heating liquid
  2. customAbsorption of oxygen

Sources & evidence

ORD record
ord-21a75f7cba1141a9bb77acb1ac3e9d64
Source dataset
uspto-grants-1985_12
Patent number
US04558135

Linked notes

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