Phosphorus oxychloride → HCID 20531786, compound

HRID 1759352Notes

Reaction equation

HRID 1759352 reaction equation
CN(C)C(=O)C.[CH2:7]([N:9]([CH2:33][CH3:34])[C:10]1[CH:15]=[CH:14][C:13]([N:16]=[N:17][C:18]2[CH:23]=[CH:22][C:21]([O:24][CH2:25][CH2:26][O:27][CH3:28])=[C:20]([S:29](O)(=[O:31])=[O:30])[CH:19]=2)=[CH:12][CH:11]=1)[CH3:8].P(Cl)(Cl)([Cl:37])=O>C(#N)C>[CH2:7]([N:9]([CH2:33][CH3:34])[C:10]1[CH:15]=[CH:14][C:13]([N:16]=[N:17][C:18]2[CH:23]=[CH:22][C:21]([O:24][CH2:25][CH2:26][O:27][CH3:28])=[C:20]([S:29]([Cl:37])(=[O:31])=[O:30])[CH:19]=2)=[CH:12][CH:11]=1)[CH3:8]

Participants

5

Reactant 3

HCID 24813Phosphorus oxychlorideHCID 31374DimethylacetamideHCID 20531785HCID 20531785, compound

Product 1

HCID 20531786HCID 20531786, compound

Reagents, catalysts & solvents 1

HCID 6342AcetonitrileSolvent

Conditions

Temperature
30 °C

Procedure

10 ml of N,N-dimethylacetoamide was added dropwise to a mixture of 13 g of N,N-diethyl-4-[4-(2-methoxyethoxy)-3-sulfophenylazo]-aniline prepared in Step (1) described above, 100 ml of acetonitrile and 13 ml of phosphorus oxychloride while the reaction mixture was maintained at a temperature of 30° C. or lower. After completion of the addition, the mixture was allowed to stand with stirring over a period of 3 hours and then, it was poured little by little into 500 ml of ice water. The crystals thus precipitated were recovered by filtration, washed with 200 ml of water and air-dried. Yield 11.0 g, Melting Point 103°-104° C.

Workup

  1. additionAfter completion of the addition
  2. customThe crystals thus precipitated
  3. filtrationwere recovered by filtration
  4. washwashed with 200 ml of water
  5. customair-dried

Sources & evidence

ORD record
ord-39f9b55392e5428cb5c3660ee62e433e
Source dataset
uspto-grants-1982_07
Patent number
US04340661

Reaction notes

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