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tert-Butyl piperazine-1-carboxylate → Tert-butyl 4-(3-nitropyridin-4-yl)piperazine-1-carboxylate

HRID 2066613
ノート
印刷プレビュー

反応式

HRID 2066613 の反応式
[N+:1]([C:4]1[CH:5]=[N:6][CH:7]=[CH:8][C:9]=1Cl)([O-:3])=[O:2].C(N(CC)C(C)C)C.[C:19]([N:26]1[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]1)([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:20]>ClCCl>[C:22]([O:21][C:19]([N:26]1[CH2:31][CH2:30][N:29]([C:9]2[CH:8]=[CH:7][N:6]=[CH:5][C:4]=2[N+:1]([O-:3])=[O:2])[CH2:28][CH2:27]1)=[O:20])([CH3:25])([CH3:23])[CH3:24]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 143452tert-Butyl piperazine-1-carboxylateHCID 521913N,N-Diethyl-2-propanamineHCID 27357814-Chloro-3-nitropyridine

生成物 1

HCID 59332343Tert-butyl 4-(3-nitropyridin-4-yl)piperazine-1-carboxylate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

3-Nitro-4-Chloro pyridine (10 mmol) dissolved in dichloromethane (25 mL) and diethyl iso propyl amine (20 mmol) followed Boc piperazine(10 mmol) was added to the above solution while cooling at 0° C. and the reaction mixture was stirred at room temperature for overnight . The dichloromethane was evaporated under vacuum. The resulting solid is extracted in to dichloromethane and washed with citric acid and brine solution. The evaporation of dichloromethane gave a yellow solid, 4-(3-Nitro-pyridin-4-yl)-piperazine-1-carboxylic acid tert-butyl ester which is used for next step without purification.

後処理

  1. additionwas added to the above solution
  2. customThe dichloromethane was evaporated under vacuum
  3. extractionThe resulting solid is extracted in to dichloromethane
  4. washwashed with citric acid and brine solution
  5. customThe evaporation of dichloromethane

出典と根拠

ORDレコード
ord-995d34cb4cd3417ca37b0837391ee486
出典データセット
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08293747B2

反応ノート

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