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Water → tert-Butyl 4-(6-chloro-5-nitropyrimidin-4-yl)piperazine-1-carboxylate

HRID 2112895
ノート
印刷プレビュー

反応式

HRID 2112895 の反応式
Cl[C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[C:6]([Cl:11])[N:5]=[CH:4][N:3]=1.[C:12]([O:16][C:17]([N:19]1[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]1)=[O:18])([CH3:15])([CH3:14])[CH3:13].C(N(CC)CC)C.O>C(#N)C>[C:12]([O:16][C:17]([N:19]1[CH2:24][CH2:23][N:22]([C:2]2[C:7]([N+:8]([O-:10])=[O:9])=[C:6]([Cl:11])[N:5]=[CH:4][N:3]=2)[CH2:21][CH2:20]1)=[O:18])([CH3:15])([CH3:13])[CH3:14]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 203124,6-Dichloro-5-nitropyrimidineHCID 143452tert-Butyl piperazine-1-carboxylate

生成物 1

HCID 21477639tert-Butyl 4-(6-chloro-5-nitropyrimidin-4-yl)piperazine-1-carboxylate

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

4,6-Dichloro-5-nitropyrimidine [CAS No. 4316-93-2] (2.0 g) was dissolved in acetonitrile (30 mL), and then piperazine-1-carboxylic acid t-butyl ester (1.92 g) and triethylamine (2.1 mL) were added to this solution. The reaction solution was stirred at room temperature for 14 hours, and then water (30 mL) was added. The reaction solution was stirred at room temperature for 30 minutes, and then the precipitate was collected by filtration. The obtained solid was washed with water and hexane to give the title compound (2.94 g).

後処理

  1. stirringThe reaction solution was stirred at room temperature for 30 minutes
  2. filtrationthe precipitate was collected by filtration
  3. washThe obtained solid was washed with water and hexane

出典と根拠

ORDレコード
ord-dde78d0f2ba34eb5be44adc5a029b910
出典データセット
uspto-grants-2009_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07524847B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート