반응 #44793

ord-bb0e708cf4c14bd1beb626c6497cc125

반응 방정식

O=C([O-])O
bicarbonate
c1ccc(COc2ccc(CN3CCCNCC3)cc2)cc1
hexahydro-1-[[4-(phenylmethoxy)phenyl]methyl]-1H-1,4-diazepine
COC(=O)CCCBr
methyl 4-bromobutanoate
CCN(CC)CC
triethylamine
COC(=O)CCCN1CCCN(Cc2ccc(OCc3ccccc3)cc2)CC1
methyl hexahydro-4-[[4-(phenylmethoxy)phenyl]methyl]-1H-1,4-diazepine-1-butanoate
수율 79.7%

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도the reaction was heated
  2. 2
    온도at reflux for 4 hours
  3. 3
    온도to cool
  4. 4
    세척The combined ethyl acetate extracts were washed with water
  5. 5
    기타dried
  6. 6
    농축concentrated

실험 절차

In a manner similar as described above in Paragraph A, a solution of hexahydro-1-[[4-(phenylmethoxy)phenyl]methyl]-1H-1,4-diazepine (150 mg, 0.506 mmol) and methyl 4-bromobutanoate (0.29 mL, 2.0 mmol) in THF (6 mL) was treated with triethylamine (0.28 mL, 2 mmol) and the reaction was heated at reflux for 4 hours. The reaction was allowed to cool and treated with an aqueous bicarbonate solution. The combined ethyl acetate extracts were washed with water, dried and concentrated to give 0.16 g of methyl hexahydro-4-[[4-(phenylmethoxy)phenyl]methyl]-1H-1,4-diazepine-1-butanoate.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07737145B2uspto-grants-2010_06