Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Formaldehyde | HCID 712 | — |
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Reactant | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| Reactant | HCID 11252029 | HCID 11252029 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 11321022 | HCID 11321022 | 85.8% |
Reaction Steps
At 22° C., 22.4 g (0.746 mol) of paraformaldehyde were added with stirring, over a period of 2 min to a mixture of 100 g (0.746 mol) of methyl N-amino-N-2-hydroxyethylcarbamate in 1500 ml of methylene chloride. After addition of 8.5 g (0.045 mol) of p-toluenesulfonic acid, the mixture was stirred at 42° C. for 21 h, until the precipitate had dissolved, and was then cooled to 20° C., and magnesium sulfate was added. The mixture was filtered and the filtrate was concentrated under reduced pressure. This gave 111.8 g of the title compound as a colorless resin with a GC purity of 85%, corresponding to a yield of 85.8% of theory.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06639070B1 |
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| Source dataset | uspto-grants-2003_10 |
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| ORD ID | ord-9b5668dcceb848afbe17850441d57acc |
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| Source note | uspto-grants-2003_10 |
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