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Dimethylformamide → 2-(6-Bromopyridin-3-yl)acetonitrile

HRID 889291
ノート
印刷プレビュー

反応式

HRID 889291 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8]Cl)=[CH:4][N:3]=1.[CH3:10][N:11](C=O)C.[C-]#N.[Na+].[Cl-].[NH4+]>C(OCC)(=O)C>[Br:1][C:2]1[N:3]=[CH:4][C:5]([CH2:8][C:10]#[N:11])=[CH:6][CH:7]=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 4

HCID 6228DimethylformamideHCID 8929Sodium CyanideHCID 25517Ammonium ChlorideHCID 64246582-Bromo-5-(chloromethyl)pyridine

生成物 1

HCID 177499762-(6-Bromopyridin-3-yl)acetonitrile

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

3.75 g (18.2 mmol) of the compound from Example 6A are initially introduced into 20 ml DMF, 979 mg (20.0 mmol) sodium cyanide are added and the mixture is stirred at RT for 2 d. The reaction mixture is introduced on to a mixture of 250 ml saturated ammonium chloride solution and 200 ml ethyl acetate and the aqueous phase is extracted with ethyl acetate (three times with 100 ml each time). The combined organic phases are dried over sodium sulfate, filtered and concentrated and the residue is dried in vacuo. The product obtained in this way is reacted without further purification.

後処理

  1. additionare added
  2. extractionthe aqueous phase is extracted with ethyl acetate (three times with 100 ml each time)
  3. dry with materialThe combined organic phases are dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customthe residue is dried in vacuo
  7. customThe product obtained in this way
  8. customis reacted without further purification

出典と根拠

ORDレコード
ord-a969a42e32974f22b6062135daa58f5a
出典データセット
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08252817B2

反応ノート

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