Phosphorus oxide (P4O10) → HCID 13290183, compound

HRID 652629Notes

Reaction equation

HRID 652629 reaction equation
O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O.[Cl:15][C:16]1[C:21]([Cl:22])=[C:20]([O:23][CH3:24])[CH:19]=[CH:18][C:17]=1[S:25][CH:26]1[CH2:31][CH2:30][CH2:29][CH2:28][C:27]1=O>O>[Cl:22][C:21]1[C:20]([O:23][CH3:24])=[CH:19][C:18]2[C:27]3[CH2:28][CH2:29][CH2:30][CH2:31][C:26]=3[S:25][C:17]=2[C:16]=1[Cl:15]

Participants

4

Reactant 2

HCID 14812Phosphorus oxide (P4O10)HCID 13290208HCID 13290208, compound

Product 1

HCID 13290183HCID 13290183, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

A mixture of "super" polyphosphoric acid is freshly prepared by mixing 7.0 g of phosphorous pentoxide and 40 g of polyphosphoric acid. The mixture is heated to 135°-140° and, with efficient stirring, is added 5.5 g of finely pulverized 2-[2,3-dichloro-4-methoxyphenylthio]cyclohexanone. Stirring is continued at 140° for 2 hours and the mixture is cooled, diluted with water and filtered. The crude product is filtered, air-dried and purified by passing it through a silica column. Elution with ether-hexane (50:50) yields 4.3 g of 3,4-dichloro-6,7,8,9-tetrahydro-2-methoxydibenzothiophene as off-white crystals, mp 123°-125°.

Workup

  1. customis freshly prepared
  2. temperatureThe mixture is heated to 135°-140° and, with efficient stirring
  3. temperaturethe mixture is cooled
  4. filtrationfiltered
  5. filtrationThe crude product is filtered
  6. customair-dried
  7. custompurified
  8. washElution with ether-hexane (50:50)

Sources & evidence

ORD record
ord-f72cb81d477c4806ad23c44980ca769d
Source dataset
uspto-grants-1987_06
Patent number
US04672138

Reaction notes

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