HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triphenylphosphine → Methyl 4-{[[(2,4-dinitrophenyl)sulfonyl]({1-[(trimethylsilyl)methyl]-1H-1,2,3-triazol-4-yl}methyl)amino]methyl}benzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | Diethyl azodicarboxylate | HCID 5462977 | — |
| Reactant | (1-((Trimethylsilyl)methyl)-1h-1,2,3-triazol-4-yl)methanol | HCID 59627317 | — |
| Reactant | Methyl 4-({[(2,4-dinitrophenyl)sulfonyl]amino}methyl)benzoate | HCID 59627340 | — |
| Solvent | Benzene | HCID 241 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | Methyl 4-{[[(2,4-dinitrophenyl)sulfonyl]({1-[(trimethylsilyl)methyl]-1H-1,2,3-triazol-4-yl}methyl)amino]methyl}benzoate | HCID 59627272 | — |
Reaction Steps
A solution of {1-[(trimethylsilyl)methyl]-1H-1,2,3-triazol-4-yl}methanol (241 mg, 1.30 mmol), methyl 4-({[(2,4-dinitrophenyl)sulfonyl]amino}methyl)benzoate (514 mg, 1.30 mmol), triphenylphosphine (409 mg, 1.56 mmol) and benzene (4.34 mL) was treated with diethylazodicarboxylate (247 uL, 1.56 mmol). After one hour additional portions of triphenylphosphine (204 mg, 0.780 mmol) and diethylazodicarboxylate (124 uL, 0.780 mmol) The reaction was diluted with EtOAc and washed with 2M aq. HCl 2×, water, brine, dried (MgSO4) and concentrated to afford a brown oil used crude in the next reaction. MS: cal'd 563 (MH+), exp 563 (MH+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09096559B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-fbd65a37cabb4723994529d43b4a7427 |
| Source note | uspto-grants-2015_08 |