HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 57945508, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | N-Hydroxysuccinimide | HCID 80170 | — |
| Reactant | HCID 57945497 | HCID 57945497 | — |
| Solvent | Dimethylacetamide | HCID 31374 | — |
| Product | HCID 57945508 | HCID 57945508 | 35% |
Reaction Steps
2-(dimethylamino)-4-(pyridin-2-yldisulfanyl)butanoic acid (218) (92 mg, 0.338 mmol), 1-hydroxypyrrolidine-2,5-dione (65 mg, 0.565 mmol) and EDC (185 mg, 0.965 mmol) was stirred in 3 ml of DMA at 50° C. overnight. The mixture was evaporated and purified on a SiO2 column eluted with from 1:10 to 1:4 of methanol/CH2Cl2 to afford 43 mg (35%) of the title product. 1H NMR (CDl3OD) 8.40 (m, 1H), 7.83 (m, 2H), 7.22 (m, 1H), 3.34 (m, 1H), 2.82 (m, 2H), 2.75 (s, 4H), 2.66 (s, 6H), 1.98 (m, 2H); 13C NMR 177.21, 161.78, 161.12, 150.68, 139.37, 122.70, 121.66, 70.80, 44.16, 43.15, 36.06, 27.38; ESI MS m/z+369.2 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08236319B2 |
| Source dataset | uspto-grants-2012_08 |
| ORD ID | ord-e8c5bc4adebc47e18c340d2d2f8a70da |
| Source note | uspto-grants-2012_08 |