Chlorine monoxide → HCID 9992152, compound

HRID 261013Notes

Reaction equation

HRID 261013 reaction equation
O=[C:2]1[NH:8][C:7]2[CH:9]=[CH:10][CH:11]=[CH:12][C:6]=2[S:5][C:4]2[N:13]=[CH:14][CH:15]=[CH:16][C:3]1=2.O(Cl)[Cl:18].P(Cl)(Cl)(Cl)(Cl)Cl>>[Cl:18][C:2]1[C:3]2[CH:16]=[CH:15][CH:14]=[N:13][C:4]=2[S:5][C:6]2[CH:12]=[CH:11][CH:10]=[CH:9][C:7]=2[N:8]=1

Participants

4

Reactant 3

HCID 24646Chlorine monoxideHCID 24819Phosphorus pentachlorideHCID 14976083HCID 14976083, compound

Product 1

HCID 9992152HCID 9992152, compound

Procedure

40 G 5,6-DIHYDRO-5-OXOPYRIDO[2,3-B][1,5]BENZOTHIAZEPINE ARE ADDED TO A MIXTURE OF 200 CM3PHOSPHORUS OXYCHLORIDE AND 71 G PHOSPHORUS PENTACHLORIDE. The reaction mixture is heated under reflux for 4 hours, then the excess phosphorus oxychloride is eliminated by distillation. The residue is then taken up in 300 cm3 cold chloroform. The organic solution is washed several times with iced water, then dried over magnesium sulphate. The solvents are eliminated by distillation under vacuum at ambient temperature. The residue is taken up in anhydrous ether, then washed several times with cold ether. After drying under vacuum, 37 g 5-chloropyrido[2,3-b][1,5]benzothiazepine are obtained, having a melting point of 134°-135° C.

Workup

  1. temperatureThe reaction mixture is heated
  2. temperatureunder reflux for 4 hours
  3. distillationthe excess phosphorus oxychloride is eliminated by distillation
  4. washThe organic solution is washed several times with iced water
  5. dry with materialdried over magnesium sulphate
  6. distillationThe solvents are eliminated by distillation under vacuum at ambient temperature
  7. washwashed several times with cold ether
  8. dry with materialAfter drying under vacuum, 37 g 5-chloropyrido[2,3-b][1,5]benzothiazepine
  9. customare obtained

Sources & evidence

ORD record
ord-30f8b7fff2c5476586a3482d94acd2ca
Source dataset
uspto-grants-1979_08
Patent number
US04163785

Reaction notes

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