Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Phosgene | HCID 6371 | — |
| Reactant | HCID 22475658 | HCID 22475658 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 12151506 | HCID 12151506 | — |
Reaction Steps
N-Methyl-N-(2-methacryloyloxyethyl)amine hydrochloride (95.0 g, 0.529 mol) produced in Example 1 was suspended in methylene chloride (300 ml) and heated to 50° C. Phosgene (7.85 g, 0.793 mol) was introduced into the resultant suspension over two hours. The resultant reaction mixture was further stirred for one hour, and then the methylene chloride was removed from the mixture to produce N-methyl-N-(2-methacryloyloxyethyl)carbamoyl chloride (106.6 g, almost quantitative yield, purity: 98%) as a colorless transparent liquid. The product was analyzed through gas chromatography (column: silicone SE-30 20% glass column (2 m), injection temperature: 220° C., detection temperature: 230° C.). FIGS. 3 and 4 show the infrared spectrum and NMR spectrum of the product, respectively.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06646156B2 |
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| Source dataset | uspto-grants-2003_11 |
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| ORD ID | ord-127672a56e5f4f6dae5f858ba2c96500 |
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| Source note | uspto-grants-2003_11 |
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