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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Isopropyl Benzoate → ethyl 3-(1-((2S,3aR,6aR)-3a-((S,4S)-5-(4-(trifluoromethyl)pyridin-2-yl)-2,5-diazabicyclo[2.2.1]heptane-2-carbonyl)octahydropentalen-2-yl)piperidin-4-yl)benzoate

HRID 1400074
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HRID 1400074 반응식
[F:1][C:2]([F:28])([F:27])[C:3]1[CH:8]=[CH:7][N:6]=[C:5]([N:9]2[CH2:14][C@@H:13]3[CH2:15][C@H:10]2[CH2:11][N:12]3[C:16]([C@@:18]23[CH2:25][CH2:24][CH2:23][C@@H:22]2[CH2:21][C:20](=O)[CH2:19]3)=[O:17])[CH:4]=1.[NH:29]1[CH2:34][CH2:33][CH:32]([C:35]2[CH:36]=[C:37]([CH:43]=[CH:44][CH:45]=2)[C:38]([O:40][CH2:41][CH3:42])=[O:39])[CH2:31][CH2:30]1.[BH4-].[Na+].C(=O)(O)[O-].[Na+].C(OC(C)C)(=O)C1C=CC=CC=1>ClC(Cl)C.CC(C)[O-].[Ti+4].CC(C)[O-].CC(C)[O-].CC(C)[O-].CO>[F:28][C:2]([F:27])([F:1])[C:3]1[CH:8]=[CH:7][N:6]=[C:5]([N:9]2[CH2:14][C@@H:13]3[CH2:15][C@H:10]2[CH2:11][N:12]3[C:16]([C@@:18]23[CH2:25][CH2:24][CH2:23][C@@H:22]2[CH2:21][C@H:20]([N:29]2[CH2:34][CH2:33][CH:32]([C:35]4[CH:36]=[C:37]([CH:43]=[CH:44][CH:45]=4)[C:38]([O:40][CH2:41][CH3:42])=[O:39])[CH2:31][CH2:30]2)[CH2:19]3)=[O:17])[CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 5

HCID 13654Isopropyl BenzoateHCID 516892Sodium BicarbonateHCID 4311764Sodium borohydrideHCID 57880398Ethyl 3-(piperidin-4-yl)benzoateHCID 89823414(3aR,6aR)-3a-((1S,4S)-5-(4-(trifluoromethyl)pyridin-2-yl)-2,5-diazabicyclo[2.2.1]heptane-2-carbonyl)hexahydropentalen-2(1H)-one

생성물 1

HCID 86698132
ethyl 3-(1-((2S,3aR,6aR)-3a-((S,4S)-5-(4-(trifluoromethyl)pyridin-2-yl)-2,5-diazabicyclo[2.2.1]heptane-2-carbonyl)octahydropentalen-2-yl)piperidin-4-yl)benzoate

시약·촉매·용매 3

HCID 11026Titanium isopropoxide촉매HCID 887Methanol용매HCID 63651,1-Dichloroethane용매

실험 절차

A mixture of Example 9E (200 mg, 0.5 mmol), ethyl 3-(piperidin-4-yl)benzoate (125 mg, 0.56 mmol) in dichloroethane (20 mL) was added titanium(IV) isopropoxide (0.6 ml, 2.03 mmol) at room temperature. The mixture was stirred at room temperature for 12 hours. Sodium borohydride (96.7 mg, 2.54 mmol) and methanol (1 mL) were added to the reaction mixture and stirred for another 2 hours. LC-MS indicated that the reaction was complete. Aqueous Sodium bicarbonate (20 mL) was added to the reaction mixture. The reaction mixture was extracted with dichloromethane (3×30 mL). The organic fractions were dried with sodium sulfate, filtered, and concentrated. The residue was purified by chromatography (eluent: 20 to 80% ethylacetate in petroleum ether) on silica to give a mixture of the title compound and isopropyl benzoate.

후처리

  1. stirringstirred for another 2 hours
  2. extractionThe reaction mixture was extracted with dichloromethane (3×30 mL)
  3. dry with materialThe organic fractions were dried with sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe residue was purified by chromatography (eluent: 20 to 80% ethylacetate in petroleum ether) on silica
  7. customto give

출처 및 근거

ORD 기록
ord-fe7e532311b34cbb8636b2921fb2e7a1
출처 데이터셋
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08906911B2

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