HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium iodide → HCID 54712214, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium iodide | HCID 66321 | — |
| Reactant | HCID 58739071 | HCID 58739071 | — |
| Solvent | 2,4,6-Trimethylpyridine | HCID 7953 | — |
| Product | HCID 54712214 | HCID 54712214 | 76% |
Reaction Steps
Reaction of 2-(1,1-dioxo-1λ6-[1,2]thiazinan-2-yl)-5-methoxy-1-methyl-6-oxo-1,6-dihydro-pyrimidine-4-carboxylic acid 3,4-dichloro-benzylamide (0.160 g, 0.337 mmol) in 2,4,6-collidine with lithium iodide gave 0.118 g (76% yield) of the title amide as a white solid. 1HNMR 400 MHz (CDCl3) δ (ppm): 1.70–1.85 and 2.06–2.15 (2×1H, 2 m, CH2), 2.3–2.4 (2H, m, CH2), 3.2–3.33 (2H, m, CH2 ), 3.64 (3H, s, NCH3), 3.7–3.85 (2H, m, CH2), 4.58 (2H, AB part of ABX system, JAB=15.5 Hz, Δν=49.6 Hz, JAX=6.6 Hz, JBX=6.1 Hz, NCH2), 7.18 (1H, broad dd, aromatic), 7.42 (1H, broad d, aromatic), 7.45 (1H, d, J=8.1 Hz, aromatic, 7.57 (1H, broad NH). HRMS (FAB POS) calculated for C17H19Cl2N4O5S [M+H+]: 461.045322. found: 461.045599.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07135467B2 |
| Source dataset | uspto-grants-2006_11 |
| ORD ID | ord-e225515cce964b60a07216e4e2986f56 |
| Source note | uspto-grants-2006_11 |