HCID 13065291, compound → HCID 13065292, compound

HRID 1995653Notes

Reaction equation

HRID 1995653 reaction equation
[CH3:1][O:2][C:3]1[CH:12]=[C:11]([NH:13]C(C)=O)[C:10]([S:17]([OH:20])(=[O:19])=[O:18])=[CH:9][C:4]=1[C:5]([O:7][CH3:8])=[O:6]>CO>[CH3:1][O:2][C:3]1[CH:12]=[C:11]([NH2:13])[C:10]([S:17]([OH:20])(=[O:19])=[O:18])=[CH:9][C:4]=1[C:5]([O:7][CH3:8])=[O:6]

Participants

3

Reactant 1

HCID 13065291HCID 13065291, compound

Product 1

HCID 13065292HCID 13065292, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

75 liters of methanol is placed in a 100 liter reactor. It is agitated and 24.5 kg of finely ground methyl 2-methoxy-4-acetamino-5-sulfobenzoate is added. The sulfonic acid dissolves; the deacetylated derivative crystallises shortly afterwards. The reaction mixture is left at room temperature for 24 hours, with agitation, so as to complete precipitation. The product is drained in a centrifugal drier, washed twice, with 6 liters of methyl alcohol each time, and dried in a ventilated oven at 50° C.; it has the following properties:

Workup

  1. customthe deacetylated derivative crystallises shortly afterwards
  2. washwashed twice, with 6 liters of methyl alcohol each time
  3. customdried in a ventilated oven at 50° C.

Sources & evidence

ORD record
ord-05072a656d844a4b9140fba0a8c91545
Source dataset
uspto-grants-1983_09
Patent number
US04405636

Reaction notes

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