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2-Chloro-3-nitropyridine → tert-Butyl (1-(3-nitropyridin-2-yl)piperidin-4-yl)carbamate

HRID 2233835
ノート
印刷プレビュー

反応式

HRID 2233835 の反応式
[C:1]([O:5][C:6](=[O:14])[NH:7][CH:8]1[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1)([CH3:4])([CH3:3])[CH3:2].Cl[C:16]1[C:21]([N+:22]([O-:24])=[O:23])=[CH:20][CH:19]=[CH:18][N:17]=1>CN1C(=O)CCC1>[N+:22]([C:21]1[C:16]([N:11]2[CH2:12][CH2:13][CH:8]([NH:7][C:6](=[O:14])[O:5][C:1]([CH3:4])([CH3:2])[CH3:3])[CH2:9][CH2:10]2)=[N:17][CH:18]=[CH:19][CH:20]=1)([O-:24])=[O:23]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 796132-Chloro-3-nitropyridineHCID 7238334-(N-Boc-amino)piperidine

生成物 1

HCID 44120582tert-Butyl (1-(3-nitropyridin-2-yl)piperidin-4-yl)carbamate収率 83.8%

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

Anhydrous TEA (0.76 ml, 5.49 mmol) was added to piperidin-4-yl-carbamic acid tert-butyl ester (1 g, 5 mmol) and 2-chloro-3-nitro-pyridine (0.791 g, 5 mmol) in anhydrous NMP (3 ml). Using a Smith Microwave Synthesizer, the mixture was subjected to single-mode microwave at 150° C. for 10 minutes. The brown solution was partitioned between EtOAc and water and the organic phase was washed several times with water, dried over sodium sulphate and concentrated in vacuo to give the title compound as a yellow solid (1.35 g).

後処理

  1. customat 150° C.
  2. customfor 10 minutes
  3. customThe brown solution was partitioned between EtOAc and water
  4. washthe organic phase was washed several times with water
  5. dry with materialdried over sodium sulphate
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-3fa3454866764ee1a3b191f0da1e0b2e
出典データセット
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07709503B2

反応ノート

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