HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → HCID 71625873, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Oxalyl chloride | HCID 65578 | — |
| Reactant | HCID 71625747 | HCID 71625747 | — |
| Reactant | HCID 71625872 | HCID 71625872 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 71625873 | HCID 71625873 | 80% |
Reaction Steps
Following the method used to prepare 24a, the use of 53 (0.35 g, 0.96 mmol) and oxalyl chloride (120 μL, 1.44 mmol) followed by allowing the intermediate acid chloride to react with ammonia in dioxane provided 0.28 g (80%) of product 24b as an off white solid, mp 197° C. 1H NMR (300 MHz, DMSO-d6) δ 2.40 (s, 3H), 3.70 (s, 2H), 6.90 (d, J=8 Hz, 1H), 6.99-7.01 (m, 2H), 7.08 (brs, 1H), 7.20 (d, J=8 Hz, 1H), 7.25-7.28 (m, 2H), 7.54 (brs, 1H), 11.65 (brs, 1H). LC-MS (CI): m/z 365.0, 367.0 [(M+H)+ C17H14Cl2NO2S requires 364.0]. Purity (100%). Calcd for C17H14Cl2NO2S: C, 55.90; H, 3.86; N, 7.67; S, 8.78; Cl, 19.41. Found: C, 55.61; H, 3.90; N, 7.68; S, 8.59; Cl, 19.67.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09233921B2 |
| Source dataset | uspto-grants-2016_01 |
| ORD ID | ord-e234154716494b2b84c40faa3b6ebada |
| Source note | uspto-grants-2016_01 |