Trifluoroacetic acid → 3-(Piperidin-4-ylmethyl)pyridine

HRID 862737ノート

反応式

HRID 862737 の反応式
CC(C)(OC([N:7]1[CH2:12][CH2:11][CH:10]([CH2:13][C:14]2[CH:15]=[N:16][CH:17]=[CH:18][CH:19]=2)[CH2:9][CH2:8]1)=O)C.FC(F)(F)C(O)=O.[OH-].[Na+]>C(Cl)(Cl)Cl>[N:16]1[CH:17]=[CH:18][CH:19]=[C:14]([CH2:13][CH:10]2[CH2:11][CH2:12][NH:7][CH2:8][CH2:9]2)[CH:15]=1

参加物

5

反応物 3

HCID 6422Trifluoroacetic acidHCID 14798Sodium HydroxideHCID 185388801-(1,1-Dimethylethyloxycarbonyl)-4-(3-pyridylmethyl)piperidine

生成物 1

HCID 37932203-(Piperidin-4-ylmethyl)pyridine収率 95%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

A solution of 1-(1,1-dimethylethyloxycarbonyl)-4-(3-pyridylmethyl)piperidine (500 mg, 1.80 mmol) in chloroform (14 mL) was cooled to 0° C. and treated with trifluoroacetic acid (5 mL, 65.14 mmol). The resulting mixture was stirred for 1 h and then made basic by addition of aqueous sodium hydroxide. The organic extracts were separated and the aqueous was reextracted three more times with chloroform. The chloroform extracts were combined, dried over sodium sulfate, filtered and concentrated on a rotary evaporator to give the title compound as a colorless oil (300 mg, 1.70 mmol, 95%).

後処理

  1. customThe organic extracts were separated
  2. dry with materialdried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated on a rotary evaporator

出典と根拠

ORDレコード
ord-fb6be0b8edce460b8568a5637de71777
出典データセット
uspto-grants-1998_02
特許番号
US05719166

反応ノート

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