Methanesulfonic Acid → HCID 135593842, compound

HRID 1391390Notes

Reaction equation

HRID 1391390 reaction equation
CS(O)(=O)=[O:3].[OH-].[NH4+].O[C:9]1[CH:10]=[CH:11][CH:12]=[C:13]([C:15]2[S:19][C:18]([NH:20][C:21](=[O:32])[C:22]3[C:27]([O:28][CH3:29])=[CH:26][CH:25]=[CH:24][C:23]=3[O:30][CH3:31])=[N:17][N:16]=2)[CH:14]=1>>[OH:3][C:10]1[CH:11]=[CH:12][C:13]([C:15]2[S:19][C:18]([NH:20][C:21](=[O:32])[C:22]3[C:27]([O:28][CH3:29])=[CH:26][CH:25]=[CH:24][C:23]=3[O:30][CH3:31])=[N:17][N:16]=2)=[CH:14][CH:9]=1

Participants

4

Reactant 3

HCID 6395Methanesulfonic AcidHCID 14923Ammonium HydroxideHCID 12881496HCID 12881496, compound

Product 1

HCID 135593842HCID 135593842, compound

Procedure

The residue produced above was stirred, and 20 g. of methanesulfonic acid was added dropwise to it. After 4 hours of stirring, at room temperature, the solution was poured into 300 ml. of ice water, and the pH was adjusted with ammonium hydroxide to 7.5. A precipitate separated, which was collected and recrystallized from acetone to produce 2.5 g. of N-[5-(5-hydroxyphenyl)-1,3,4-thiadiazol-2-yl]-2,6-dimethoxybenzamide, m.p. above 260°.

Workup

  1. customThe residue produced
  2. stirringAfter 4 hours of stirring, at room temperature
  3. additionthe solution was poured into 300 ml
  4. customA precipitate separated
  5. customwhich was collected
  6. customrecrystallized from acetone
  7. customto produce 2.5 g

Sources & evidence

ORD record
ord-a8b405b499a84ca185b67c0aa547b0ff
Source dataset
uspto-grants-1979_02
Patent number
US04141984

Reaction notes

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