Phosphorus oxychloride → HCID 57419393, compound

HRID 1990917Notes

Reaction equation

HRID 1990917 reaction equation
[ClH:1].[CH3:2][C:3]1[NH:18][C:6]2[N:7]=[C:8]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[N:9]=[C:10](O)[C:5]=2[CH:4]=1.P(Cl)(Cl)([Cl:21])=O>O>[ClH:21].[Cl:1][C:10]1[C:5]2[CH:4]=[C:3]([CH3:2])[NH:18][C:6]=2[N:7]=[C:8]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[N:9]=1

Participants

4

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 178422240HCID 178422240, compound

Product 1

HCID 57419393HCID 57419393, compoundYield 97%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

A heterogeneous mixture of 4 (4.0 g, 17.76 mmol) and phosphorus oxychloride (125 mL) was heated to reflux. After 14 h the homogeneous solution was cooled to room temperature and concentrated in vacuo yielding a black oil. Water was added to the oil and the mixture was warmed. The resulting solid was filtered, washed with water and dried at room temperature to yield 4.22 g of a brown solid (97%). 1H NMR (200 MHz, DMSO-d6): δ 2.43 (s, 3H), 6.31 (s, 1H), 7.49 (m, 3H), 8.34 (m, 2H).

Workup

  1. temperaturewas heated to reflux
  2. concentrationconcentrated in vacuo
  3. customyielding a black oil
  4. temperaturethe mixture was warmed
  5. filtrationThe resulting solid was filtered
  6. washwashed with water
  7. customdried at room temperature

Sources & evidence

ORD record
ord-61fa616c4dfe4dfa888933432bf275d2
Source dataset
uspto-grants-2010_01
Patent number
US07645754B2

Reaction notes

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