Carbamic acid,N-[3-[(methylsulfonyl)amino]propyl]-, 1,1-dimethylethyl ester synthesis
- Product Name:Carbamic acid,N-[3-[(methylsulfonyl)amino]propyl]-, 1,1-dimethylethyl ester
- CAS Number:1204669-77-1
- Molecular formula:C9H20N2O4S
- Molecular Weight:252.3311
Yield:1204669-77-1 95%
Reaction Conditions:
with triethylamine in tetrahydrofuran at 0; for 1.5 h;
Steps:
58.1 Step 1: tert-Butyl (3-(methylsulfonamido)propyl)carbamate (69)
To a solution of tert-butyl-3-aminopropyl-carbamate (68) (1.07 g, 5.8 mmol) in anhydrous THF (15 mL) was added triethylamine (1.2 mL, 8.7 mmol) and the mixture was cooled to 0C. Methane sulfonyl chloride (0.64 mL, 8.2 mmol) was added and the mixture was stirred at 0oC for 1.5 h. The solvent was removed under reduced pressure, and the resulting residue was diluted with EtOAc and washed with water. The aqueous layer was back-extracted with EtOAc three times. The organic layers were combined and washed with saturated brine, and dried over sodium sulfate and filtered. The solvent was evaporated to obtain the title compound (69) (1.45 g, 95%) as a solid which was used directly.
References:
WO2018/39621,2018,A1 Location in patent:Paragraph 00356-00357
75178-96-0
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