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Diethyl Ether → HCID 70564665, 화합물

HRID 1427261
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HRID 1427261 반응식
[C:1]([O:5][C:6]([NH:8][C:9]1[CH:17]=[CH:16][CH:15]=[C:14]2[C:10]=1[CH:11]=[CH:12][N:13]2[C:18]([C:25]1[CH:30]=[CH:29][C:28]([Cl:31])=[CH:27][CH:26]=1)([CH2:23][CH3:24])[C:19](OC)=[O:20])=[O:7])([CH3:4])([CH3:3])[CH3:2].[CH2:32]([Mg]Br)[CH3:33].CCOCC.C(=O)(O)[O-].[Na+]>C1COCC1.CC(=O)OCC.CC(C)[O-].[Ti+4].CC(C)[O-].CC(C)[O-].CC(C)[O-]>[Cl:31][C:28]1[CH:29]=[CH:30][C:25]([C:18]([N:13]2[C:14]3[C:10](=[C:9]([NH:8][C:6](=[O:7])[O:5][C:1]([CH3:2])([CH3:4])[CH3:3])[CH:17]=[CH:16][CH:15]=3)[CH:11]=[CH:12]2)([C:19]2([OH:20])[CH2:33][CH2:32]2)[CH2:23][CH3:24])=[CH:26][CH:27]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 3283Diethyl EtherHCID 516892Sodium BicarbonateHCID 70560825HCID 70560825, 화합물HCID 178418443HCID 178418443, 화합물

생성물 1

HCID 70564665HCID 70564665, 화합물

시약·촉매·용매 3

HCID 11026Titanium isopropoxide촉매
HCID 8028
Tetrahydrofuran
용매
HCID 8857Ethyl Acetate용매

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온도
0 °C

실험 절차

To a solution of methyl 2-{4-[(tert-butoxycarbonyl)amino]-1H-indol-1-yl}-2-(4-chlorophenyl)butanoate (0.44 g, 1 mmol), as described in Example 3 step A, in THF (20 mL) was added titanium (IV) isopropoxide (0.3 g, 1 mmol) and the solution was cooled to 0° C. Ethylmagnesium bromide 3 N in ether (1.8 mL, 5 mmol) was then added via syringe pump over 1 hr period and the reaction was stirred for an additional 30 min at this temperature. The mixture was warmed into RT and stirred over night. The final mixture was diluted with EA, treated with saturated sodium bicarbonate solution, extracted with EA and DCM, dried over sodium sulfate and concentrated. The residue was purified by flash-chromatography over silica gel (eluted with hexanes/EA 95:5 to EA) to give the title compound. LC/MS m/z=441.0[M+H]+.

후처리

  1. temperatureThe mixture was warmed into RT
  2. stirringstirred over night
  3. extractionextracted with EA and DCM
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated
  6. customThe residue was purified by flash-chromatography over silica gel (eluted with hexanes/EA 95:5 to EA)

출처 및 근거

ORD 기록
ord-30d4db862ee84c28abe4bb94299fa929
출처 데이터셋
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08933113B2

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