Phosphorus pentachloride → HCID 68844946, compound

HRID 2109019Notes

Reaction equation

HRID 2109019 reaction equation
[C:1]([N:4]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[C:6](=[C:13](O)[C:14]2[CH:19]=[CH:18][C:17]([NH:20][C:21](=[O:23])[CH3:22])=[C:16]([N+:24]([O-:26])=[O:25])[CH:15]=2)[C:5]1=[O:28])(=[O:3])[CH3:2].P(Cl)(Cl)(Cl)(Cl)[Cl:30]>O1CCOCC1>[C:1]([N:4]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[C:6](=[C:13]([Cl:30])[C:14]2[CH:19]=[CH:18][C:17]([NH:20][C:21](=[O:23])[CH3:22])=[C:16]([N+:24]([O-:26])=[O:25])[CH:15]=2)[C:5]1=[O:28])(=[O:3])[CH3:2]

Participants

4

Reactant 2

HCID 24819Phosphorus pentachloride2×HCID 178474214HCID 178474214, compound

Product 1

HCID 68844946HCID 68844946, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Conditions

Temperature
100 °C

Procedure

A suspension of 11.4 g of 1-acetyl-3-(1-hydroxy-1-(4-acetylamino-3-nitro-phenyl)methylene)-2-indolinone (educt VII.21) and 9.37 g of phosphorus pentachloride in 200 ml dioxane is stirred for 4 hours at 100° C. After the addition of a further 2.0 g of phosphorus pentachloride the mixture is stirred for a further 3 hours at 100° C. Then the solvent is distilled off, the residue is stirred with 100 ml of ethyl acetate, suction filtered, washed with ethyl acetate and dried at 60° C.

Workup

  1. stirringis stirred for a further 3 hours at 100° C
  2. distillationThen the solvent is distilled off
  3. stirringthe residue is stirred with 100 ml of ethyl acetate, suction
  4. filtrationfiltered
  5. washwashed with ethyl acetate
  6. customdried at 60° C.

Sources & evidence

ORD record
ord-f14e541fb69c463ebd7914469b9a53c6
Source dataset
uspto-grants-2009_04
Patent number
US07514468B2

Reaction notes

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