반응 #307237

ord-afc8319216b54771bfc39a25664dbb30

반응 방정식

O
water
CCN(CC)CC
triethylamine
Cl.O=S1(=O)CCNCC1
thiomorpholine 1,1-dioxide hydrochloride
O=C(Cl)Oc1ccc([N+](=O)[O-])cc1
4-nitrophenyl chloroformate
O=C(Oc1ccc([N+](=O)[O-])cc1)N1CCS(=O)(=O)CC1
4-Nitrophenyl thiomorpholine-4-carboxylate 1,1-dioxide

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도while cooling with an ice bath
  2. 2
    여과filtered
  3. 3
    기타The residue was dried under high vacuum

실험 절차

17.0 g (99.2 mmol) of thiomorpholine 1,1-dioxide hydrochloride were initially charged in 100 ml of dichloromethane and, while cooling with an ice bath, admixed with 20.7 ml (15.1 g, 148.8 mmol) of triethylamine. 10.0 g (49.6 mmol) of 4-nitrophenyl chloroformate were added in portions. The reaction mixture was stirred at RT for 30 minutes, admixed with water and ethyl acetate and then filtered. The residue was dried under high vacuum. Yield: 12.4 g (83% of theory)

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08202862B2uspto-grants-2012_06