반응 #42279

ord-7583b3517ea042a9a2c4d870052b9855

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타solvent is then removed
  2. 2
    기타The residue is partitioned between ethyl acetate and water
  3. 3
    기타The organic phase is separate
  4. 4
    세척washed with saline
  5. 5
    건조dried over anhydrous sodium sulfate
  6. 6
    여과filtered
  7. 7
    농축concentrated

실험 절차

To a solution of methyl 3-(chlorosulfonyl)-5-[(dipropylamino)carbonyl]benzoate (XXXVII, PREPARATION 11, 0.100 g, 0.300 mmol) in dry THF (3 mL) is added ammonia (7 N solution in methanol, 0.214 mL, 1.50 mmol). The mixture is stirred for 18 hours and solvent is then removed. The residue is partitioned between ethyl acetate and water. The organic phase is separate and washed with saline, dried over anhydrous sodium sulfate, filtered, and concentrated to give the title compound, NMR (300 MHz, CDCl3) delta 8.45, 8.07, 8.01, 6.05, 3.93, 3.44, 3.09, 1.67, 1.52, 0.96 and 0.73; MS (ESI+) for C12H22N2O5S m/z (M+H)+=343.3.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07727997B2uspto-grants-2010_06