HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 178479375, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | 1-Butanol | HCID 263 | — |
| Reactant | Boron Trichloride | HCID 25135 | — |
| Reactant | 1-Nitro-3-(n,n'-bis(tert-butyloxycarbonyl)guanidino)benzene | HCID 69871752 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178479375 | HCID 178479375 | 62% |
Reaction Steps
To a stirred solution of compound 17 (238 milligrams, 0.492 millimoles) in CH2Cl2 was added 1.97 milliliters of 1 molar BCl3 (1.97 millimoles) in CH2Cl2. After 30 minutes, excess BCl3 and CH2Cl2 were removed by passing a stream of nitrogen gas across the surface of the solution. The resulting material was washed with CH2Cl2. The product was obtained as a white powder in 62% yield. TLC (4:1:1 n-butanol:acetic acid:water) indicated a single spot that was also UV active (Rf=0.47). 1H-NMR (DMSO): δ7.6-7.8 (m, 3H), 8.0-8.15 (m, 1H), 10.25 (brs.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06387890B1 |
| Source dataset | uspto-grants-2002_05 |
| ORD ID | ord-802cfeb82c674db3b9d5f33671f6eabe |
| Source note | uspto-grants-2002_05 |