HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → Methyl 4-methoxy-2-sulfamoylbenzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Methyl 2-(chlorosulfonyl)-4-methoxybenzoate | HCID 13769571 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Methyl 4-methoxy-2-sulfamoylbenzoate | HCID 13769572 | 25.3% |
Reaction Conditions
| Temperature | -10 °C |
|---|
Reaction Steps
A solution of 554 g of the compound of Example 4 in 5 L of dichloromethane was cooled to -40° C. and 79 g of anhydrous ammonia was added at this temperature. The reaction mixture was allowed to warm to -10° C., stirred 1 hour, then poured into 6 L of water. The organic phase was separated and filtered. The filter cake was washed with dichloromethane and dried giving 356 g of crude product. A 180 g portion was recrystallized from methanol to give 130 g of the title compound, m.p. 139°-142° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04632693 |
| Source dataset | uspto-grants-1986_12 |
| ORD ID | ord-cc175d25fd0140b590023b0642c12631 |
| Source note | uspto-grants-1986_12 |