HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triphenylphosphine → HCID 54537267, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| Reactant | Ethyl 2-(4-hydroxyphenyl)-2-oxoacetate | HCID 11715332 | — |
| Reactant | 3-[4-(2-Chlorophenyl)-9-methyl-6H-thieno[3,2-f][1,2,4]triazolo[4,3-a][1,4]diazepin-2-yl]prop-2-yn-1-ol | HCID 15084135 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 54537267 | HCID 54537267 | 73% |
Reaction Steps
As in Example 15, 4-(-2-chlorophenyl)-2-(3-hydroxy-1-propynyl)-9-methyl-6H-thieno[3,2-f][1,2,4]triazolo[4,3-a][1,4]diazepine (0.369 g) was reacted with 4-hydroxyphenylglyoxylic acid ethyl ester (0.195 g) in the presence of diethyl azodicarboxylate (0.175 g) and triphenylphosphine (0.263 g) in dichloromethane (30 mL). The crude reaction product, isolated in the usual manner, was purified by flash chromatography over silica gel (120 g; ethanol-dichloromethane; 3.5:96.5) to furnish 0.398 g of 4-[3-[4-(2-chlorophenyl)-9-methyl-6H-thieno[3,2-f][1,2,4]triazolo[4,3-a] [1,4]diazepin-2-yl]-2-propynyloxy]-alpha-oxobenzeneacetic acid ethyl ester (4:1 ) hydrate as a white foam.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05344843 |
| Source dataset | uspto-grants-1994_09 |
| ORD ID | ord-032a1707c72c4fef9e3b2d5d60042e11 |
| Source note | uspto-grants-1994_09 |