HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 178462812, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | 2-(4-Chlorophenyl)-2-propynoic acid | HCID 18607 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | HCID 23504692 | HCID 23504692 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 178462812 | HCID 178462812 | 21% |
Reaction Steps
To the solution of 190 mg (1 mmol) of (4-chlorophenyl)-propargylic acid in 20 ml of DMF at 0° C. is added 165 mg (1.1 mmol) of HOBT and 210 mg (1.1 mmol) of EDC. After 3 h at 0° C., 367 mg (1 mmol) of 4-[6-(3-Amino-phenylamino)-9-ethyl-9H-purin-2-ylamino]-cyclohexanol (example 77, stage 1.2) is added. After 1 h at 0° C. and 2.5 h at RT, the solvent was removed under reduced pressure. The crude product is purified by means of column chromatography on silica gel, trituration in diethyl ether and recrystallisation from ethanol to obtain 110 mg (0.21 mmol) of N-{3-[9-Ethyl-2-(trans-4-hydroxy-cyclohexylamino)-9H-purin-6yl-amino]-phenyl}-3-(4-chlorophenyl)-propargylic acid amide.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06767906B2 |
| Source dataset | uspto-grants-2004_07 |
| ORD ID | ord-09a13aa4c3644918948888d8bc4e2169 |
| Source note | uspto-grants-2004_07 |