Methylamine → HCID 178482323, compound

HRID 1076546Notes

Reaction equation

HRID 1076546 reaction equation
[CH3:1][NH2:2].[Cl:3][C:4]1[NH:5][SH:6](=[O:25])([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[C:7]2[CH:13]=[C:12]([S:14](=[O:17])(=[O:16])[NH2:15])[C:11]([Cl:18])=[CH:10][C:8]=2[N:9]=1>C(COC)OC>[ClH:3].[Cl:18][C:11]1[C:12]([S:14](=[O:17])(=[O:16])[NH2:15])=[CH:13][C:7]2[SH:6](=[O:25])([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[NH:5][C:4]([NH:2][CH3:1])=[N:9][C:8]=2[CH:10]=1

Participants

4

Reactant 2

HCID 6329MethylamineHCID 178514677HCID 178514677, compound

Product 1

HCID 178482323HCID 178482323, compound

Reagents, catalysts & solvents 1

HCID 80711,2-DimethoxyethaneSolvent2×

Procedure

To a stirred mixture of 5.14 g. (0.066 mole) of 40% aqueous methylamine solution and 50 ml. of glyme is added, over a 30 minute period, a solution of 13.5 g. (0.035 mole) of 3,6-dichloro-1-phenyl-7-sulfamyl-1,2,4-benzothiadiazine -1-oxide in 150 ml. of glyme. The reaction mixture is heated under reflux for 10 hours, cooled, concentrated to dryness, and suspended in 100 ml. of 10% hydrochloric acid. Filtration of the solid material yields the product.

Workup

  1. additionTo a stirred mixture of 5.14 g
  2. temperatureThe reaction mixture is heated
  3. temperatureunder reflux for 10 hours
  4. temperaturecooled
  5. concentrationconcentrated to dryness
  6. filtrationFiltration of the solid material
  7. customyields the product

Sources & evidence

ORD record
ord-a24628213b5543b3a95fa803fe238bb4
Source dataset
uspto-grants-1976_05
Patent number
US03957769

Reaction notes

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