Phosphorus oxychloride → HCID 86722242, compound

HRID 869393Notes

Reaction equation

HRID 869393 reaction equation
O[C:2]1[CH:7]=[C:6]([C:8]2[N:9]=[C:10]([CH:13]([CH3:15])[CH3:14])[S:11][CH:12]=2)[N:5]=[C:4]2[C:16]3[C:22]([Cl:23])=[C:21]([O:24][CH3:25])[CH:20]=[CH:19][C:17]=3[O:18][C:3]=12.O=P(Cl)(Cl)[Cl:28]>>[Cl:28][C:2]1[CH:7]=[C:6]([C:8]2[N:9]=[C:10]([CH:13]([CH3:15])[CH3:14])[S:11][CH:12]=2)[N:5]=[C:4]2[C:16]3[C:22]([Cl:23])=[C:21]([O:24][CH3:25])[CH:20]=[CH:19][C:17]=3[O:18][C:3]=12

Participants

3

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 178488262HCID 178488262, compound

Product 1

HCID 86722242HCID 86722242, compound

Procedure

The crude 10C (8.75 g, 23.34 mmol) was added to POCl3 (200 mL) The mixture was refluxed for 2 hours. TLC monitored the reaction. After the reaction completed, POCl3 was evaporated under reduced pressure. The residue was poured into crushed ice under stirring. The yellow solids were collected by filtration and purified by flash chromatography to give product M10 (0.66 g).

Workup

  1. temperaturewas refluxed for 2 hours
  2. customthe reaction
  3. customPOCl3 was evaporated under reduced pressure
  4. additionThe residue was poured
  5. custominto crushed ice
  6. filtrationThe yellow solids were collected by filtration
  7. custompurified by flash chromatography
  8. customto give product M10 (0.66 g)

Sources & evidence

ORD record
ord-a8a8e91967864ef4b21bc3073a0eac08
Source dataset
uspto-grants-2015_03
Patent number
US08969373B2

Reaction notes

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