HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hexane → HCID 178466034, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hexane | HCID 8058 | — |
| Reactant | HCID 69850080 | HCID 69850080 | — |
| Solvent | 1,1'-Biphenyl, mixt. with 1,1'-oxybis(benzene) | HCID 24670 | — |
| Product | HCID 178466034 | HCID 178466034 | — |
Reaction Steps
A sample of 2-cyano-3-(6-ethoxy-pyridin-3-ylamino)-acrylic acid ethyl ester was heated at 257-259° C. (internal temperature) in Dowtherm for 10-12 hrs under nitrogen. After cooling, the reaction mixture was poured into n-hexane. The black solid was collected, and treated with MeOH and CH2Cl2 mixture (1:5). The title compound (or tautomer) was collected and dried mass spectrum (electrospray, m/e): 215.9 (M+H); IR cm-1: 3063, 2226; H-NMR δ(DMSO-d6): 1.355 (3H, t, CH3), 4.412 (2H, q, CH2), 7.244 (1H, d, C7-H), 7.983 (1H, d, C8-H), 8.682 (1H, s, C2-H), 10.50 (1H, bs, OH).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06355636B1 |
| Source dataset | uspto-grants-2002_03 |
| ORD ID | ord-aca15010ec9b4596b5495c0666a81c7b |
| Source note | uspto-grants-2002_03 |