4-Nitrophenol → 1-[3-(4-Nitrophenoxy)propyl]piperidine

HRID 495449노트

반응식

HRID 495449 반응식
Cl[CH2:2][CH2:3][CH2:4][N:5]1[CH2:10][CH2:9][CH2:8][CH2:7][CH2:6]1.[N+:11]([C:14]1[CH:19]=[CH:18][C:17]([OH:20])=[CH:16][CH:15]=1)([O-:13])=[O:12].C([O-])([O-])=O.[K+].[K+]>CN(C=O)C.O.CCOC(C)=O>[N+:11]([C:14]1[CH:19]=[CH:18][C:17]([O:20][CH2:2][CH2:3][CH2:4][N:5]2[CH2:10][CH2:9][CH2:8][CH2:7][CH2:6]2)=[CH:16][CH:15]=1)([O-:13])=[O:12]

참가 물질

7

반응물 3

HCID 9804-NitrophenolHCID 11430Potassium CarbonateHCID 79625Piperidine, 1-(3-chloropropyl)-

생성물 1

HCID 20579281-[3-(4-Nitrophenoxy)propyl]piperidine

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

In a three-neck flask with an overhead mechanical stirrer, a mixture of 1-(3-chloropropyl)-piperidine (49.8 g, 0.308 mol), 4-nitrophenol (42.8 g, 0.308 mol) and K2CO3 (212 g, 1.53 mol), in anhydrous DMF (200 mL) was heated to 94° C. and stirred for 18 h. The mixture was cooled to RT then diluted with 2 L water. The organics were taken up in EtOAc (2 L) and washed twice with 2N NaOH (500 mL) then brine (200 mL). The combined organics were dried over anhydrous MgSO4 then concentrated under reduced pressure to give 1-[3-(4-nitro-phenoxy)-propyl]-piperidine as a yellowish oil.

후처리

  1. washwashed twice with 2N NaOH (500 mL)
  2. dry with materialThe combined organics were dried over anhydrous MgSO4
  3. concentrationthen concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-4bd0f96b7d594befaebf83a55e4816a7
출처 데이터셋
uspto-grants-2005_09
특허 번호
US06939874B2

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