Dimethylformamide → HCID 73665042, compound

HRID 2309200Notes

Reaction equation

HRID 2309200 reaction equation
CN(C)C=O.[Cl:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]2[S:17][C:16]([SH:18])=[N:15][N:14]=2)=[CH:9][CH:8]=1.[OH-].[K+].[F:21][C:22]([F:29])([F:28])[C:23]([F:27])=[C:24](F)[F:25]>C(Cl)(Cl)Cl>[F:25][C:24]([S:18][C:16]1[S:17][C:13]([C:10]2[CH:9]=[CH:8][C:7]([Cl:6])=[CH:12][CH:11]=2)=[N:14][N:15]=1)=[C:23]([F:27])[C:22]([F:29])([F:28])[F:21]

Participants

6

Conditions

Temperature
60 °C

Procedure

60 ml of dimethylformamide and 6.85 g of 5-(4-chlorophenyl)-2-mercapto-1,3,4-thiadiazole and 0.7 g of potassium hydroxide are stirred in an autoclave. 20 g of hexafluoropropylene are pressed in, and the reaction mixture is heated for 19 hours at 60° C. (10-12·105Pa). After cooling and release of pressure, the solution is poured into ice-water, the product is taken up in chloroform, the chloroform solution is washed with 1n sodium hydroxide solution, and the solvent is removed in vacuo, affording as reside the title compound in the form of an crystals with a melting point of 69°-70° C.

Workup

  1. temperatureAfter cooling
  2. washthe chloroform solution is washed with 1n sodium hydroxide solution
  3. customthe solvent is removed in vacuo

Sources & evidence

ORD record
ord-60c5b464fada400eac84567af63c4503
Source dataset
uspto-grants-1987_09
Patent number
US04694014

Reaction notes

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