Water → HCID 23362013, compound

HRID 1082060Notes

Reaction equation

HRID 1082060 reaction equation
P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:2].[F:15][C:16]([F:34])([F:33])[C:17]1[CH:32]=[CH:31][C:20]2[C:21](=O)[NH:22][C:23]3[CH2:29][CH2:28][CH:27]=[CH:26][C:24]=3[S:25][C:19]=2[CH:18]=1.O>N1C=CC=CC=1>[F:15][C:16]([F:34])([F:33])[C:17]1[CH:32]=[CH:31][C:20]2[C:21](=[S:2])[NH:22][C:23]3[CH:29]=[CH:28][CH:27]=[CH:26][C:24]=3[S:25][C:19]=2[CH:18]=1

Participants

5

Reactant 3

HCID 962WaterHCID 14817Phosphorus sulfide (P2S5)HCID 54556120HCID 54556120, compound

Product 1

HCID 23362013HCID 23362013, compoundYield 106.6%

Reagents, catalysts & solvents 1

HCID 1049PyridineSolvent

Procedure

Phosphorus pentasulphide (2.25 g) was added to a solution of 3-trifluoromethyl-9,10-dihydrodibenzo [b,f][1,4]thiazepin-11-one (2 g, 6.8 mmol) in pyridine (30 ml) and the mixture heated under reflux for 6.5 hr. The mixture was allowed to cool and then poured into warm water (100 ml) with stirring. Filtration of the cooled mixture and recrystallisation from ethanol gave the title compound as yellow needles (1.68 g, m.p. 236°-239° C., Rf 0.58, hexane/EtOAc 2:1).

Workup

  1. temperaturethe mixture heated
  2. temperatureunder reflux for 6.5 hr
  3. temperatureto cool
  4. additionpoured
  5. filtrationFiltration of the cooled mixture and recrystallisation from ethanol

Sources & evidence

ORD record
ord-b1adc63d70f6411799925c012b321fd2
Source dataset
uspto-grants-1996_12
Patent number
US05589474

Reaction notes

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