HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → HCID 86675066, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 2-(Thiophen-2-yl)-1,3-thiazole-4-carboxylic acid | HCID 2776317 | — |
| Reactant | HCID 86675067 | HCID 86675067 | — |
| Product | HCID 86675066 | HCID 86675066 | — |
Reaction Steps
To Intermediate 4-Amino-3-[9-(2,2,2-trifluoro-acetyl)-2,9-diaza-spiro[5.5]undec-2-yl]-benzonitrile was added 2-thiophen-2-yl-thiazole-4-carboxylic acid (098 eq) in DMF (1 mL). Then, a solution of N,N-diisopropylethylamine (1.5 eq) HATU (1.5 eq) was added. The resulting reaction was stirred at room temperature for 15 hours and then concentrated and treated with 3 mL of (4:1) TFA:H2SO4. The reaction mixture was concentrated and purified using reverse phase HPLC to provide 2-Thiophen-2-yl-thiazole-4-carboxylic acid {4-carbamoyl-2-[9-(2,2,2-trifluoro-acetyl)-2,9-diaza-spiro[5.5]undec-2-yl]-phenyl}-amide. HPLC-MS RT=4.46 min, mass calculated for formula C26H26F3N5O3S2 577.14, observed LCMS m/z 578.21 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09206142B2 |
| Source dataset | uspto-grants-2015_12 |
| ORD ID | ord-918e10c3dd114ad697d6741e7d1f49cd |
| Source note | uspto-grants-2015_12 |