Methane → HCID 20097216, compound

HRID 1769626Notes

Reaction equation

HRID 1769626 reaction equation
Cl[C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[N:4]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][N:12]=2)[CH:3]=1.P(=O)(O)(O)[OH:18].C>COCCO>[N:12]1[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=1[N:4]1[C:5]2[C:10](=[CH:9][CH:8]=[CH:7][CH:6]=2)[CH2:2][C:3]1=[O:18]

Participants

5

Reactant 3

HCID 297MethaneHCID 1004Phosphoric AcidHCID 20097208HCID 20097208, compound

Product 1

HCID 20097216HCID 20097216, compound

Reagents, catalysts & solvents 1

HCID 80192-MethoxyethanolSolvent

Conditions

Temperature
100 °C

Procedure

Dissolve the 3-chloro-1-(pyrid-2-yl)-indole in 1500 cm3 of 2-methoxyethanol and heat to 100° C. with stirring. Add 1100 cm3 of 70% phosphoric acid in a fine stream. Continue heating for 6 hours and then treat the reaction mixture with charcoal under reflux for 15 mins. Filter. Heat to 70° C. while adding 2000 cm3 of water. Cool the precipitated product for 12 hours at 5° C. Filter and dry.

Workup

  1. temperatureContinue heating for 6 hours
  2. temperatureunder reflux for 15 mins
  3. filtrationFilter
  4. temperatureHeat to 70° C.
  5. additionwhile adding 2000 cm3 of water
  6. temperatureCool the precipitated product for 12 hours at 5° C
  7. filtrationFilter
  8. customdry

Sources & evidence

ORD record
ord-ee7fa3cd0aa244bd803d717aca3bd80c
Source dataset
uspto-grants-1995_01
Patent number
US05382593

Reaction notes

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