HuagongsheHuagongshe Chemistry Print Report · For research reference only
Formaldehyde → 4-{[(4-tert-Butyl-phenyl)-(4-iodo-phenylcarbamoyl)-methyl]-methyl-amino}-benzoic Acid Tert-butyl Ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Formaldehyde | HCID 712 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Sodium cyanoborohydride | HCID 5003444 | — |
| Reactant | 4-{[(4-tert-Butyl-phenyl)-(4-iodo-phenylcarbamoyl)-methyl]-amino}-benzoic Acid Tert-butyl Ester | HCID 67486559 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | 4-{[(4-tert-Butyl-phenyl)-(4-iodo-phenylcarbamoyl)-methyl]-methyl-amino}-benzoic Acid Tert-butyl Ester | HCID 67486343 | 105.5% |
Reaction Steps
4-{[(4-tert-Butyl-phenyl)-(4-iodo-phenylcarbamoyl)-methyl]-amino}-benzoic acid tert-butyl ester (110 mg, 0.19 mmol) was dissolved in 2 mL of HOAc. paraformaldehyde (51 mg, 0.57 mmol) and sodium cyano-borohydride (36 mg, 0.57 mmol) were then added and heated to 40 C for 1 h. Cooled to RT, EtOAc (20 mL) was added and extracted water (20 mL). The organic layer was washed again with water (20 mL), dried over sodium sulfate, filtered and the organic layer was removed under reduced pressure to give a white solid (120 mg, 100%). 1H NMR showed the compound to be very clean and sufficient for the following step. LCMS (M+1=599.4)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08710236B2 |
| Source dataset | uspto-grants-2014_04 |
| ORD ID | ord-4efc979011514c6b862ad26c81d10acb |
| Source note | uspto-grants-2014_04 |