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

HRID 1042698ノート

反応式

HRID 1042698 の反応式
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.C(OCC)(=O)C>[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]

参加物

7

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

In a three-necked flask fitted 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 potassium carbonate (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 room temperature, then diluted with 2 L water. The organics were taken up in ethyl acetate and washed twice with 2N sodium hydroxide and then brine. The combined organics were dried over magnesium sulfate then concentrated under reduced pressure to give the title compound as a yellowish oil.

後処理

  1. customIn a three-necked flask fitted with an overhead mechanical stirrer
  2. washwashed twice with 2N sodium hydroxide
  3. dry with materialThe combined organics were dried over magnesium sulfate
  4. concentrationthen concentrated under reduced pressure

出典と根拠

ORDレコード
ord-52da004ae7ee4932be4af4a614801a3f
出典データセット
uspto-grants-2013_10
特許番号
US08557996B2

反応ノート

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