Ethanol → HCID 18441772, 화합물

HRID 458155

반응식

HRID 458155 반응식
[CH2:1]([N:8]1[C:12](=[O:13])[C:11]2([CH2:18][CH2:17][NH:16][CH2:15][CH2:14]2)[N:10]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl[CH:26]1[CH2:31][CH2:30][CH2:29][CH2:28][CH2:27]1.C(N(CC)CC)C.C([OH:41])C>>[CH2:1]([N:8]1[C:12](=[O:13])[C:11]2([CH2:18][CH2:17][N:16]([CH:27]3[CH2:28][CH2:29][CH2:30][CH2:31][C:26]3=[O:41])[CH2:15][CH2:14]2)[N:10]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

5

반응물 4

HCID 702EthanolHCID 8471TriethylamineHCID 10952ChlorocyclohexaneHCID 184417443-Benzyl-1-phenyl-1,3,8-triazaspiro[4.5]decan-4-one

생성물 1

HCID 18441772HCID 18441772, 화합물

실험 절차

A solution of 0.30 g (0.93 mmol) 3-benzyl-1-phenyl-1,3,8-triaza-spiro[4.5]decan-4-one, 0.14 g (1.0 mmol) 2-chlorocyclohexane, and 0.2 ml (1.4 mmol) triethylamine in ethanol was refluxed overnight. The reaction mixture was cooled to ambient temperature, concentrated and then quenched with saturated NaHCO3 and extracted with ethyl acetate. The combined organic extracts were washed with brine, dried over MgSO4, filtered and evaporated. Purification of the crude product over a silica gel plug (10:1) with n-heptane/AcOEt as eluent provided 0.14 g rac-3-benzyl-8-(2-oxo-cyclohexyl)-1-phenyl-1,3,8-triaza-spiro[4.5]decan-4-one as a light yellow oil; MS (ISP): 418.4 MH+.

후처리

  1. concentrationconcentrated
  2. customquenched with saturated NaHCO3
  3. extractionextracted with ethyl acetate
  4. washThe combined organic extracts were washed with brine
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. customevaporated
  8. customPurification of the crude product over a silica gel plug (10:1) with n-heptane/AcOEt as eluent

출처 및 근거

ORD 기록
ord-36743b9b689d4a9dbc65f524433382d2
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07189850B2

연결된 노트

불러오는 중…