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1,2-Dibromoethane → 2,3-Dihydro-1,4-dioxino[2,3-b]pyridine

HRID 1038594
ノート
印刷プレビュー

反応式

HRID 1038594 の反応式
[OH:1][C:2]1[C:7]([OH:8])=[CH:6][CH:5]=[CH:4][N:3]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:16][CH2:17]Br>CN(C=O)C>[O:8]1[C:7]2[C:2](=[N:3][CH:4]=[CH:5][CH:6]=2)[O:1][CH2:17][CH2:16]1
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 78391,2-DibromoethaneHCID 11430Potassium CarbonateHCID 178516237HCID 178516237、化合物

生成物 1

HCID 110079682,3-Dihydro-1,4-dioxino[2,3-b]pyridine収率 5.7%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
90 °C

実験手順

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート

2,3-Dihydroxypyridine (2.22 g, 20.0 mmol) was dissolved in N,N′-dimethylformamide (100 mL), and added potassium carbonate (5.52 g, 40.0 mmol) at room temperature. 5 minutes after, 1,2-dibromoethane (2.6 mL, 30.0 mmol) was added at the same temperature, and stirred at 90° C. overnight. The reaction solution was reverted to room temperature, filtered, and the obtained filtrate was concentrated in vacuo. Then, the obtained residue was added ethyl acetate. The suspension was filtered, washed ethyl acetate, and concentrated in vacuo. The title compound (157 mg (yield 5.7%)) was obtained as a colorless oil.

後処理

  1. customwas reverted to room temperature
  2. filtrationfiltered
  3. concentrationthe obtained filtrate was concentrated in vacuo
  4. additionThen, the obtained residue was added ethyl acetate
  5. filtrationThe suspension was filtered
  6. washwashed ethyl acetate
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-8717438d53b14ba0aa869f0a7d640caa
出典データセット
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08551985B2

反応ノート

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