반응 #417944

ord-b05be37b5f344eb6a173e41bdea2612d

반응 방정식

CC(C)(C)OC(=O)OC(=O)OC(C)(C)C
BOC2O
C[C@H](N)c1ccc(Br)cc1
(S)-1-(4-bromophenyl)ethylamine
O=C([O-])[O-].[Na+].[Na+]
Na2CO3
C[C@H](NC(=O)OC(C)(C)C)c1ccc(Br)cc1
(S)-tert-Butyl 1-(4-bromophenyl)ethylcarbamate

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONThen the mixture is poured onto water
  2. 2
    workup.STIRRINGstirred for additional 20 min
  3. 3
    기타The layers are separated
  4. 4
    세척layer is washed with water (2×)
  5. 5
    건조dried over Na2SO4
  6. 6
    여과filtered
  7. 7
    기타the solvent is removed in vacuo

실험 절차

To 150 g (735 mmol) (S)-1-(4-bromophenyl)ethylamine in 2 L DCM are added 459 mL (918 mmol) of an aq. Na2CO3 solution (c=2 mol/L). To this mixture a solution of 164 g (749 mmol) BOC2O in 350 mL THF is added dropwise at r.t. and stirring is continued for 1 h. Then the mixture is poured onto water and stirred for additional 20 min. The layers are separated, the org. layer is washed with water (2×), dried over Na2SO4, filtered and the solvent is removed in vacuo.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08877741B2uspto-grants-2014_11