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Nitrogen → HCID 54447250, 화합물

HRID 1977904
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HRID 1977904 반응식
N#N.[CH2:3]([N:10]1[CH2:15][CH2:14][CH2:13][CH2:12][CH:11]1[CH2:16][C:17]1[CH:22]=[CH:21][C:20](Br)=[CH:19][CH:18]=1)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.C([Li])CCC.[CH3:29][C:30]1[NH:31][C:32]([CH3:41])=[CH:33][C:34]=1[C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][N:36]=1>CCCCCC.CCOCC>[CH3:29][C:30]1[NH:31][C:32]([CH3:41])=[CH:33][C:34]=1[C:35]1[CH:40]=[CH:39][CH:38]=[C:37]([C:20]2[CH:21]=[CH:22][C:17]([CH2:16][CH:11]3[CH2:12][CH2:13][CH2:14][CH2:15][N:10]3[CH2:3][C:4]3[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=3)=[CH:18][CH:19]=2)[N:36]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 947NitrogenHCID 12082743HCID 12082743, 화합물HCID 53980622HCID 53980622, 화합물HCID 178418339Butyllithium

생성물 1

HCID 54447250HCID 54447250, 화합물수율 16.2%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매2회
HCID 8058
Hexane
용매

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온도
-70 °C

실험 절차

To a 100 mL 3N round-bottomed flask equipped with septum and N2 inlet were added 175 mg (0.509 mmol) N-benzyl-2-(4-bromobenzyl)-piperidine and 7 mL dry ether. The solution was cooled to −70° C., and 0.38 mL (0.610 mmol) of a 1.6 M solution of butyl lithium in hexane added dropwise over 1 minutes. The reaction was stirred at −70° C. for 5 min, then warmed to room temperature over 20 minutes. To the stirring reaction was then added a solution of 105 mg (0.610 mmol) 2-(2,5-dimethylpyrrolyl)-pyridine in 5 mL dry ether, and the reaction, turning dark orange, was stirred at room temperature for 4 hours then quenched with aqueous ammonium chloride solution. After extraction into ethyl acetate, the organic layer was washed with brine, dried over sodium sulfate for 16 hours to effect air-oxidation to the pyridine, and evaporated. The residue was chromatographed on silica gel using methanol/methylene chloride as eluant to afford 36 mg (16%) of an oil.

후처리

  1. temperaturewarmed to room temperature over 20 minutes
  2. customTo the stirring reaction
  3. customthe reaction
  4. stirringwas stirred at room temperature for 4 hours
  5. customthen quenched with aqueous ammonium chloride solution
  6. extractionAfter extraction into ethyl acetate
  7. washthe organic layer was washed with brine
  8. dry with materialdried over sodium sulfate for 16 hours
  9. customevaporated
  10. customThe residue was chromatographed on silica gel

출처 및 근거

ORD 기록
ord-fe1ab2c3fd194bc5b2a4ce7e70c7e981
출처 데이터셋
uspto-grants-2001_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06235750B1

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