반응 #81111
ord-f0ac4d596dbe41c58ce781b429bc5435
반응 방정식
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1온도The reaction mixture was warmed at 50° C. for 5 hours
- 2온도re-cooled to -20° C.
- 3온도The reaction mixture was heated an additional 2.5 hours at 50° C.
- 4농축concentrated under reduced pressure
- 5기타to afford an amorphous solid
- 6기타The solid was triturated with ether
실험 절차
To anhydrous methanol (15 mL) at -20° C. under nitrogen was added thionyl chloride (4 mL) dropwise. The solution was allowed to warm to room temperature and then tert-Leucine (4.00 g) was added. The reaction mixture was warmed at 50° C. for 5 hours, re-cooled to -20° C. and then additional thionyl chloride (3 mL) was added dropwise. The reaction mixture was heated an additional 2.5 hours at 50° C. and then concentrated under reduced pressure and chased twice with methanol (15 mL) to afford an amorphous solid. The solid was triturated with ether to afford the title compound in 92% yield. The 300 MHz 1H NMR spectrum was found to be consistent with the proposed structure. MS (DCI/NH3) m/e 146 (M+H)+.