반응 #303886

ord-4defcdc8bc8e489dbdaa5316731a7b05

반응 방정식

CCN(CC)CC
triethylamine
BrCc1ccc(Br)cc1
4-bromobenzyl bromide
Cl.O=S1(=O)CCNCC1
thiomorpholine-1,1-dioxide hydrochloride
O=S1(=O)CCN(Cc2ccc(Br)cc2)CC1
4-(4-Bromo-benzyl)-thiomorpholine-1,1-dioxide

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타the reaction mixture is partitioned between CH2Cl2 and H2O
  2. 2
    추출The aqueous phase is re-extracted four times with CH2Cl2
  3. 3
    세척The combined organic extracts are washed with water, saturated brine
  4. 4
    건조dried over Na2SO4
  5. 5
    여과filtered
  6. 6
    농축the filtrate is concentrated in vacuo
  7. 7
    기타to afford
  8. 8
    기타after drying in HV
  9. 9
    기타the title compound which is used in the next step without further purification

실험 절차

2.18 ml (15.5 mmol) of triethylamine are added to a colorless suspension of 1.28 g (5 mmol) of 4-bromobenzyl bromide and 944 mg (5.5 mmol) thiomorpholine-1,1-dioxide hydrochloride in 15 ml DMF. After 3 h at RT, the reaction mixture is partitioned between CH2Cl2 and H2O. The aqueous phase is re-extracted four times with CH2Cl2. The combined organic extracts are washed with water, saturated brine, dried over Na2SO4, filtered and the filtrate is concentrated in vacuo to afford, after drying in HV, the title compound which is used in the next step without further purification.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08193189B2uspto-grants-2012_06