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Pyrrolidine → HCID 75480723, 화합물

HRID 2273084
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HRID 2273084 반응식
Br[C:2]1[CH:3]=[CH:4][C:5]([N+:8]([O-:10])=[O:9])=[N:6][CH:7]=1.[NH:11]1[CH2:15][CH2:14][CH2:13][CH2:12]1>O>[N+:8]([C:5]1[CH:4]=[CH:3][C:2]([N:11]2[CH2:15][CH2:14][CH2:13][CH2:12]2)=[CH:7][N:6]=1)([O-:10])=[O:9]
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참가 물질

4

반응물 2

HCID 31268PyrrolidineHCID 8176205-Bromo-2-nitropyridine

생성물 1

HCID 75480723HCID 75480723, 화합물수율 72.4%

시약·촉매·용매 1

HCID 962Water용매

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온도
120 °C

실험 절차

A mixture of 600 mg (2.93 mmol) of 5-bromo-2-nitropyridine and 1.05 g (14.63 mmol) of pyrrolidine is heated in a Biotage microwave machine for 1 hour at 120° C. The reaction medium is diluted with water and then extracted with ethyl acetate. The organic phase is washed twice with water, dried over MgSO4 and then filtered. The filtrate is evaporated under reduced pressure and then chromatographed on silica gel, eluting with a heptane/ethyl acetate mixture from (100/0 v/v) up to (50/50 v/v) to give 410 mg of 2-nitro-5-pyrrolidin-1-ylpyridine.

후처리

  1. extractionextracted with ethyl acetate
  2. washThe organic phase is washed twice with water
  3. dry with materialdried over MgSO4
  4. filtrationfiltered
  5. customThe filtrate is evaporated under reduced pressure
  6. customchromatographed on silica gel
  7. washeluting with a heptane/ethyl acetate mixture from (100/0 v/v) up to (50/50 v/v)

출처 및 근거

ORD 기록
ord-1d08bca20e5545d0b70ccbdc23196acb
출처 데이터셋
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09120812B2

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