HCID 20555895, compound → HCID 23329082, compound

HRID 895035Notes

Reaction equation

HRID 895035 reaction equation
[CH3:1][S:2][C:3]1[CH:8]=[CH:7][C:6]([S:9][C:10]2[CH:18]=[C:17]([F:19])[CH:16]=[CH:15][C:11]=2[C:12]([OH:14])=O)=[CH:5][CH:4]=1>N>[CH3:1][S:2][C:3]1[CH:4]=[CH:5][C:6]2[S:9][C:10]3[C:11](=[CH:15][CH:16]=[C:17]([F:19])[CH:18]=3)[C:12](=[O:14])[C:7]=2[CH:8]=1

Participants

3

Reactant 1

HCID 20555895HCID 20555895, compound

Product 1

HCID 23329082HCID 23329082, compound

Reagents, catalysts & solvents 1

HCID 222AmmoniaSolvent

Procedure

375 Grams of 2-(p-methylthiophenylthio)-4-fluoro-benzoic acid (Collec.Czech.Chem.Commun. 40, pg. 3523 (1975)) were heated with 2.7 kilograms of polyphosphoric acid while stirring for 3 hours at 140 degrees Centigrade. The mixture was cooled to 110 degrees Centigrade and poured into ice-water. The precipitate was sucked off, suspended in aqueous ammonia and sucked off again. After recrystallization from pyridine 200 grams of 2-methylthio-6-fluoro-9-thioxanthone was obtained as a yellow crystalline substance which melted at 135-138 degrees Centigrade.

Workup

  1. temperatureThe mixture was cooled to 110 degrees Centigrade
  2. customAfter recrystallization from pyridine 200 grams of 2-methylthio-6-fluoro-9-thioxanthone
  3. customwas obtained as a yellow crystalline substance which melted at 135-138 degrees Centigrade

Sources & evidence

ORD record
ord-47aac6a7db894f2cbb1c18536650691a
Source dataset
uspto-grants-1981_08
Patent number
US04285956

Reaction notes

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