HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Sulfite → tert-Butyl hydrogen ((4-formylphenyl)methyl)carbonimidate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Sulfite | HCID 24437 | — |
| Reactant | Triacetoxyperiodinane | HCID 159087 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | tert-Butyl [4-(hydroxymethyl)benzyl]carbamate | HCID 2794813 | — |
| Reactant | Acetone cardice | HCID 18522661 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | tert-Butyl hydrogen ((4-formylphenyl)methyl)carbonimidate | HCID 2794832 | 287.3% |
Reaction Steps
(4-Hydroxymethyl-benzyl)-carbamic acid tert-butyl ester (480 mg, 0.71 mmol) was dissolved in DCM (3 mL) and cooled to −78° C. (dry ice/acetone). Dess-Martin periodinane (331 mg, 0.78 mmol) was added to the reaction which was allowed to warm to r.t and stir for 3 h. A 1:1 solution of saturated sodium bicarbonate and sodium sulfite (20 mL) was added and the reaction mixture stirred vigorously for 15 min. The organic layer was isolated, washed with saturated sodium bicarbonate (10 mL), dried (Na2SO4) and evaporated to dryness to afford the desired compound (480 mg, 100%). m/z 258 [M++Na]+
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07939666B2 |
| Source dataset | uspto-grants-2011_05 |
| ORD ID | ord-0f966d7da61d4b9290cba7e1a90b7bdd |
| Source note | uspto-grants-2011_05 |