HuagongsheHuagongshe Chemistry Print Report · For research reference only
Citric Acid → Benzyl sulfamic acid-[6-(2-hydroxy-ethoxy)-5-(4-chlorophenyl)-4-pyrimidinyl]-amide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Citric Acid | HCID 311 | — |
| Reactant | Benzyl sulfamic acid-[6-chloro-5-(p-chloro-phenyl)-4-pyrimidinyl]-amide | HCID 21979544 | — |
| Reactant | Potassium tert-butoxide | HCID 23665647 | — |
| Solvent | Ethylene Glycol | HCID 174 | — |
| Product | Benzyl sulfamic acid-[6-(2-hydroxy-ethoxy)-5-(4-chlorophenyl)-4-pyrimidinyl]-amide | HCID 21979542 | — |
Reaction Conditions
| Temperature | 102 °C |
|---|
Reaction Steps
Potassium tert.-butoxide (3.5 g) was dissolved in ethyleneglycol (35 ml), benzyl sulfamic acid-[6-chloro-5-(4-chlorophenyl)-4-pyrimidinyl]-amide (1.8 g, Referential Example 15) was added and the mixture was heated to 102° C. for 11 h. The mixture was poured onto ice/water and acidified to pH=4 with solid citric acid. The precipitated product was filtered off, washed with water and dried at HV to give benzyl sulfamic acid-[6-(2-hydroxy-ethoxy)-5-(4-chlorophenyl)-4-pyrimidinyl]-amide (1.77 g). tR=4.36 (LC); [M+H]+=435.09 (ES+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07285549B2 |
| Source dataset | uspto-grants-2007_10 |
| ORD ID | ord-a25d3fb25e584c9a889fabd6c803785b |
| Source note | uspto-grants-2007_10 |