Methanol → HCID 20083167, compound

HRID 1609084Notes

Reaction equation

HRID 1609084 reaction equation
S(Cl)(Cl)=O.[F:5][C:6]1[C:7]([OH:24])=[C:8]2[C:13]3=[C:14]([C:16](=[O:22])[C:17]([C:19]([OH:21])=[O:20])=[CH:18][N:12]3[N:11]([CH3:23])[CH2:10][CH2:9]2)[CH:15]=1.[CH3:25]O>>[F:5][C:6]1[C:7]([OH:24])=[C:8]2[C:13]3=[C:14]([C:16](=[O:22])[C:17]([C:19]([O:21][CH3:25])=[O:20])=[CH:18][N:12]3[N:11]([CH3:23])[CH2:10][CH2:9]2)[CH:15]=1

Participants

4

Reactant 3

HCID 887MethanolHCID 24386Thionyl ChlorideHCID 20083102HCID 20083102, compound

Product 1

HCID 20083167HCID 20083167, compound

Procedure

To 100 ml of methanol, while cooling on ice, 9 ml of thionyl chloride was added, and the solution was stirred for 30 minutes at the same temperature. 2.60 g of the compound (166) obtained in Example 43 was added to the solution, and the solution was heated at reflux for 24 hours. After air-cooling, insoluble matter was removed by filtering, and the filtrate was removed by distillation. To the residue, chloroform was added, and the formed solid matter was filtered off to obtain 2.20 g of the subject compound (167).

Workup

  1. additionwas added
  2. temperaturethe solution was heated
  3. temperatureat reflux for 24 hours
  4. temperatureAfter air-cooling
  5. custominsoluble matter was removed
  6. filtrationby filtering
  7. customthe filtrate was removed by distillation
  8. additionTo the residue, chloroform was added
  9. filtrationthe formed solid matter was filtered off

Sources & evidence

ORD record
ord-4035a4dfc0cd4581beb0ab55db63ce68
Source dataset
uspto-grants-1995_03
Patent number
US05399553

Reaction notes

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