HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Hydroxybenzoic acid hydrazide → N'-((2R,3R)-2-(3-chloro-4-cyano-2-methylphenylamino)-3-hydroxybutanoyl)-4-hydroxybenzohydrazide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Hydroxybenzoic acid hydrazide | HCID 1742 | — |
| Reactant | (2R,3R)-2-(3-chloro-4-cyano-2-methylphenylamino)-3-hydroxybutanoic acid | HCID 57908625 | — |
| Reactant | N'-((2R,3S)-2-(3-chloro-4-cyano-2-methylphenylamino)-3-hydroxybutanoyl)benzohydrazide | HCID 67006523 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | N'-((2R,3R)-2-(3-chloro-4-cyano-2-methylphenylamino)-3-hydroxybutanoyl)-4-hydroxybenzohydrazide | HCID 67006198 | 62% |
Reaction Steps
(2R,3R)-2-(3-chloro-4-cyano-2-methylphenylamino)-3-hydroxybutanoic acid (intermediate 3a) (503 mg, 1.9 mmol) was coupled with 4-hydroxy-benzohydrazide (285 mg, 1.9 mmol) similarly to the procedure described for the preparation of intermediate 1b. Trituration with hot methylene chloride provided the title compound as a white solid (380 mg, 62%). 1H NMR (500 MHz, acetone-d6, δ in ppm) 9.68 (br s, 1H), 9.30 (br s, 1H), 7.85 (AA′XX′, J=8.7 Hz, 2H), 7.52 (d, J=8.7 Hz, 1H), 6.91 (AA′XX′, J=8.8 Hz, 2H), 6.71 (d, J=8.6 Hz, 1H), 5.59 (d, J=7.1 Hz, 1H), 4.84 (br s, 1H), 4.20 (m, 1H), 4.09 (m, 1H), 2.34 (s, 3H), 1.37 (d, J=6.3 Hz, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08629167B2 |
| Source dataset | uspto-grants-2014_01 |
| ORD ID | ord-303a8eb60831411da09a8e7291bcd262 |
| Source note | uspto-grants-2014_01 |