Pyrrolidine → 3-Methoxy-5-nitro-2-(pyrrolidin-1-yl)pyridine

HRID 506506노트

반응식

HRID 506506 반응식
Cl[C:2]1[C:7]([O:8][CH3:9])=[CH:6][C:5]([N+:10]([O-:12])=[O:11])=[CH:4][N:3]=1.[NH:13]1[CH2:17][CH2:16][CH2:15][CH2:14]1>CN(C)C=O>[CH3:9][O:8][C:7]1[C:2]([N:13]2[CH2:17][CH2:16][CH2:15][CH2:14]2)=[N:3][CH:4]=[C:5]([N+:10]([O-:12])=[O:11])[CH:6]=1

참가 물질

4

반응물 2

HCID 31268PyrrolidineHCID 234561522-Chloro-3-methoxy-5-nitropyridine

생성물 1

HCID 574315163-Methoxy-5-nitro-2-(pyrrolidin-1-yl)pyridine수율 97.7%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of 3 g (15.91 mmol) of 2-chloro-3-methoxy-5-nitropyridine and 2 ml (23.86 mmol) of pyrrolidine in 30 ml of dimethylformamide is heated at 100° C. for 4 hours. The reaction mixture is subsequently concentrated under reduced pressure and then taken up in 100 ml of water and extracted three times with 100 ml of ethyl acetate. The organic phases are combined, then washed twice with 50 ml of water then once with 50 ml of a saturated sodium chloride solution, dried over sodium sulfate and then concentrated under reduced pressure. 3.47 g of the expected compound are thus isolated in the form of an orangey powder.

후처리

  1. concentrationThe reaction mixture is subsequently concentrated under reduced pressure
  2. extractionextracted three times with 100 ml of ethyl acetate
  3. washwashed twice with 50 ml of water
  4. dry with materialonce with 50 ml of a saturated sodium chloride solution, dried over sodium sulfate
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-bd838836a6014061ab81a8e94dc27ee5
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07786104B2

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