Ammonia → HCID 70455630, compound

HRID 1589297Notes

Reaction equation

HRID 1589297 reaction equation
Cl.C[O:3][C:4]1[C:9]([NH2:10])=[C:8]([NH2:11])[CH:7]=[CH:6][N:5]=1.[CH3:12][O:13][C:14]1[CH:22]=[C:21]([S:23][CH3:24])[CH:20]=[CH:19][C:15]=1[C:16](Cl)=O.N>O>[CH3:12][O:13][C:14]1[CH:22]=[C:21]([S:23][CH3:24])[CH:20]=[CH:19][C:15]=1[C:16]1[N:10]=[C:9]2[C:4](=[O:3])[NH:5][CH2:6][CH:7]=[C:8]2[N:11]=1

Participants

5

Reactant 3

HCID 222AmmoniaHCID 27595912-Methoxy-4-(methylthio)benzoyl chlorideHCID 202482542-Methoxy-3,4-diamino-pyridine hydrochloride

Product 1

HCID 70455630HCID 70455630, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

0.88 g of 2-methoxy-3,4-diamino-pyridine hydrochloride and 1.08 g of 2-methoxy-4-methylmercapto-benzoyl chloride were intimately mixed, and the mixture was stirred into warm polyphosphoric acid at 120° C. The mixture was kept at this temperature for an hour and was then poured into water, the aqueous mixture was made alkaline with ammonia, and the precipitate thus obtained was purified on a silica gel column (eluant: methylene chloride/methanol=100:10).

Workup

  1. waitThe mixture was kept at this temperature for an hour
  2. customthe precipitate thus obtained
  3. customwas purified on a silica gel column (eluant: methylene chloride/methanol=100:10)

Sources & evidence

ORD record
ord-8eb90bdb6e014f0b9d71834aa967875a
Source dataset
uspto-grants-1986_02
Patent number
US04568680

Reaction notes

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