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Sodium Chloride → 4-(tert-Butoxycarbonyl)-2,2-dimethyl-1-[4-(pyridin-4-yl)benzoyl]piperazine

HRID 352830
ノート
印刷プレビュー

反応式

HRID 352830 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][NH:11][C:10]([CH3:15])([CH3:14])[CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[N:16]1[CH:21]=[CH:20][C:19]([C:22]2[CH:30]=[CH:29][C:25]([C:26]([O-])=[O:27])=[CH:24][CH:23]=2)=[CH:18][CH:17]=1.[Cl-].[Na+]>CN(C)C=O.C(N(CC)CC)C.C(Cl)Cl>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:26](=[O:27])[C:25]2[CH:24]=[CH:23][C:22]([C:19]3[CH:18]=[CH:17][N:16]=[CH:21][CH:20]=3)=[CH:30][CH:29]=2)[C:10]([CH3:15])([CH3:14])[CH2:9]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]
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

7

反応物 3

HCID 5234Sodium ChlorideHCID 227103871-Boc-3,3-dimethylpiperazineHCID 227111444-(4-Pyridyl)benzoate

生成物 1

HCID 227107644-(tert-Butoxycarbonyl)-2,2-dimethyl-1-[4-(pyridin-4-yl)benzoyl]piperazine

試薬・触媒・溶媒 3

HCID 6228Dimethylformamide溶媒HCID 6344
Dichloromethane
溶媒
HCID 8471Triethylamine溶媒

反応条件

温度
60 °C

実験手順

To a solution of 1-(tert-butoxycarbonyl)-3,3-dimethylpiperazine (173 mg) in a mixture of N,N-dimethylformamide (2.5 ml) and triethylamine (1.0 ml) was added (4-nirophenyl) 4-(4-pyridyl)benzoate (330 mg). The resulting mixture was stirred at 60° C. for 5 days. The reaction mixture was diluted with methylene chloride and then added with a saturated aqueous solution of sodium chloride to form two layers. The organic layer obtained by separation was washed with a saturated aqueous solution of sodium bicarbonate and an aqueous solution of sodium chloride, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The crudely purified product was purified by chromatography on a silica gel column (methylene chloride:methanol=50:1), whereby the title compound (199 mg) was obtained as colorless amorphous.

後処理

  1. customto form two layers
  2. customThe organic layer obtained by separation
  3. washwas washed with a saturated aqueous solution of sodium bicarbonate
  4. dry with materialan aqueous solution of sodium chloride, dried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe crudely purified product was purified by chromatography on a silica gel column (methylene chloride:methanol=50:1), whereby the title compound (199 mg)
  7. customwas obtained as colorless amorphous

出典と根拠

ORDレコード
ord-275e5b49534645a393c00e5c79668fb3
出典データセット
uspto-grants-2004_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06747023B1

反応ノート

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