Phosphorus oxychloride → HCID 22288471, compound

HRID 968212Notes

Reaction equation

HRID 968212 reaction equation
[NH2:1][C:2]1[S:3][C:4]2[C:9](=O)[NH:8][C:7]([S:11][CH2:12][C:13]3[N:14]=[C:15]([CH3:18])[S:16][CH:17]=3)=[N:6][C:5]=2[N:19]=1.P(Cl)(Cl)([Cl:22])=O>CN(C)C1C=CC=CC=1>[Cl:22][C:9]1[C:4]2[S:3][C:2]([NH2:1])=[N:19][C:5]=2[N:6]=[C:7]([S:11][CH2:12][C:13]2[N:14]=[C:15]([CH3:18])[S:16][CH:17]=2)[N:8]=1

Participants

4

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 135555957HCID 135555957, compound

Product 1

HCID 22288471HCID 22288471, compound

Reagents, catalysts & solvents 1

HCID 949N,N-DimethylanilineSolvent

Procedure

The product from step (b), (8.7 g), was suspended in phosphorus oxychloride (88 ml) and dimethylaniline (8.8 ml). The mixture was heated under reflux for 2 hrs then evaporated. The residue was stirred in hot water, cooled and the pH adjusted with sodium hydroxide solution to pH5. The solid was collected, washed with water and dried. Chromatography (SiO2, methanol/dichloromethane as eluant) gave the sub-title compound (4.3 g)

Workup

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 2 hrs
  3. customthen evaporated
  4. temperaturecooled
  5. customThe solid was collected
  6. washwashed with water
  7. customdried

Sources & evidence

ORD record
ord-ae6d1c115f3c4cdaa6d1566edd690cd0
Source dataset
uspto-grants-2005_10
Patent number
US06958343B2

Reaction notes

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