Hydrochloric Acid → HCID 136138300, compound

HRID 615245Notes

Reaction equation

HRID 615245 reaction equation
[CH:1]1[CH:6]=[C:5]([C:7]#[N:8])[C:4]([C:9]#[N:10])=[CH:3][CH:2]=1.[Al+3:11].[Cl-].[Cl-].[Cl-].P([O-])([O-])([O-])=O.[Na+].[Na+].[Na+].Cl>O.ClC1C=CC=CC=1Cl>[Al:11].[CH:1]1[CH:2]=[CH:3][C:4]2[C:5](=[C:7]3[N:8]=[C:7]4[N:10]=[C:9]([C:4]5[CH:3]=[CH:2][CH:1]=[CH:6][C:5]=54)[N:10]=[C:9]4[NH:8][C:7]([C:5]5[CH:6]=[CH:1][CH:2]=[CH:3][C:4]=54)=[N:10][C:9]4=[N:8][C:7]([C:5]5[CH:6]=[CH:1][CH:2]=[CH:3][C:4]=54)=[N:10][C:9]=2[NH:8]3)[CH:6]=1

Participants

7

Reactant 4

HCID 313Hydrochloric AcidHCID 7042PhthalonitrileHCID 24243Trisodium PhosphateHCID 6451240Aluminum(III) Chloride

Product 1

HCID 136138300HCID 136138300, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolvent2×HCID 72391,2-DichlorobenzeneSolvent

Conditions

Temperature
75 °C

Procedure

An autoclave is charged with 128 g of phthalodinitrile, 40 g of AlCl3 and 650 g of 1,2-dichlorobenzene. After scavenging with nitrogen, the reaction mixture is heated for 26 hours to 170° C. After cooling and dearating, the suspension is stirred into 400 ml of water containing 100 g of trisodium phosphate. The batch is then evaporated to dryness in a rotary evaporator and the crude product is stirred in 750 ml of water. After addition of 60 g of 50% NaOH, heating to 75° C. and keeping this temperature for 2 hours, the crude product is isolated by filtration and the filter cake is stirred in 500 ml of water containing 80 g of 32% HCl (2 hours at 90°-95° C.). The product is filtered hot and washed, to give aluminium phthalocyanine which contains, per mole, about 1 mole of chlorine (monochloroaluminium phthalocyanine).

Workup

  1. temperaturethe reaction mixture is heated for 26 hours to 170° C
  2. temperatureAfter cooling
  3. customThe batch is then evaporated to dryness in a rotary evaporator
  4. additionAfter addition of 60 g of 50% NaOH
  5. customfor 2 hours
  6. customthe crude product is isolated by filtration
  7. filtrationThe product is filtered hot
  8. washwashed

Sources & evidence

ORD record
ord-b9f5ffea49564a99a8c19976abf6e4a3
Source dataset
uspto-grants-1985_02
Patent number
US04497741

Reaction notes

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