Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | Methanesulfonyl chloride | HCID 31297 | — |
| Edukt | tert-butyl N-(2-hydroxypropyl)carbamate | HCID 9920508 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | HCID 23134071 | HCID 23134071 | 94,2% |
Reaktionsschritte
To a solution of tert-butyl 2-hydroxypropylcarbamate (14.3 g, 81.7 mmol) and Et3N (35.6 mL, 245.1 mmol) in CH2Cl2 (250 mL) at 0° C. was slowly added a solution of methanesulfonyl chloride (9.5 mL, 122.6 mmol) in CH2Cl2 (250 mL). The mixture was stirred at 0° C. for 2 h, diluted with CH2Cl2 (300 mL) and washed with water, 1N HCl, 5% aqueous NaHCO3 and brine. The organic layer was dried over MgSO4 and concentrated under reduced pressure to afford 1-(tert-butoxycarbonylamino)propan-2-yl methanesulfonate (19.5 g, 94%) as a light yellow oil. Mass calculated for C9H19NO5S=253.32; found: [M+H]+=254.2.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08846972B2 |
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| Quelldatensatz | uspto-grants-2014_09 |
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| ORD ID | ord-49c3a7b35c7344e88e232c96323ddb1c |
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| Quellennotiz | uspto-grants-2014_09 |
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