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Chloroacetone → HCID 58351061、化合物

HRID 1477759
ノート
印刷プレビュー

反応式

HRID 1477759 の反応式
Cl[CH2:2][C:3](=[O:5])[CH3:4].[Br:6][C:7]1[N:12]=[C:11]([O:13][CH3:14])[C:10]([NH:15][CH:16]=[O:17])=[CH:9][CH:8]=1.C(=O)([O-])[O-].[Cs+].[Cs+]>CN(C=O)C.[I-].[K+]>[Br:6][C:7]1[N:12]=[C:11]([O:13][CH3:14])[C:10]([N:15]([CH2:2][C:3](=[O:5])[CH3:4])[CH:16]=[O:17])=[CH:9][CH:8]=1
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 3

HCID 6571ChloroacetoneHCID 10796Cesium carbonateHCID 71492501N-(6-bromo-2-methoxypyridin-3-yl)formamide

生成物 1

HCID 58351061HCID 58351061、化合物

試薬・触媒・溶媒 2

HCID 4875Potassium Iodide触媒HCID 6228Dimethylformamide溶媒

実験手順

Chloroactone (82 mL) was added dropwise to a suspension of N-(6-bromo-2-methoxypyridin-3-yl)formamide (159.3 g), cesium carbonate (359 g) and potassium iodide (11.4 g) IN DMF (800 mL) over seven minutes. Then, the reaction solution was stirred at room temperature for one hour and 20 minutes. The reaction solution was concentrated under reduced pressure. Ethyl acetate and water were added to the resulting residue, and the organic layer was separated. The resulting organic layer was washed with brine, dried over anhydrous magnesium sulfate and then concentrated under reduced pressure to obtain 215.2 g of the title compound. The property values of the compound are as follows.

後処理

  1. concentrationThe reaction solution was concentrated under reduced pressure
  2. additionEthyl acetate and water were added to the resulting residue
  3. customthe organic layer was separated
  4. washThe resulting organic layer was washed with brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-c0a76ea932f44446a1e433524662cd89
出典データセット
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09403815B2

反応ノート

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