Chloroform → Methyl 3-chloromethylpyrazine-2-carboxylate

HRID 2388627ノート

反応式

HRID 2388627 の反応式
[CH3:1][C:2]1[C:3]([C:8]([O:10][CH3:11])=[O:9])=[N:4][CH:5]=[CH:6][N:7]=1.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1.C(Cl)(Cl)[Cl:31]>>[Cl:31][CH2:1][C:2]1[C:3]([C:8]([O:10][CH3:11])=[O:9])=[N:4][CH:5]=[CH:6][N:7]=1

参加物

4

反応物 3

HCID 6212ChloroformHCID 7187Benzoyl PeroxideHCID 13153469Methyl 3-methylpyrazine-2-carboxylate

生成物 1

HCID 67039637Methyl 3-chloromethylpyrazine-2-carboxylate収率 52%

実験手順

Methyl 3-methylpyrazine-2-carboxylate (2.44 g, 16 mmol) was dissolved in chloroform (100 ml) and N-chlorosuccinimde (2.14 g, 16 mmol) was added thereto. Then, benzoyl peroxide (110 mg, 70%, 0.32 mmol) was added and refluxed under heating for 30 hours. The reaction solution was cooled, followed by removing undissolved substance by filtration. The filtrate was concentrated under reduced pressure, and the residue was purified by using silica gel chromatography (hexane:ethyl acetate=1:1)to obtain 1.55 g of the desired compound.

後処理

  1. additionN-chlorosuccinimde (2.14 g, 16 mmol) was added
  2. temperaturerefluxed
  3. temperatureunder heating for 30 hours
  4. temperatureThe reaction solution was cooled
  5. customby removing undissolved substance
  6. filtrationby filtration
  7. concentrationThe filtrate was concentrated under reduced pressure
  8. customthe residue was purified

出典と根拠

ORDレコード
ord-198b8725c6e9480185ee526fccd7eabb
出典データセット
uspto-grants-2012_09
特許番号
US08269045B2

反応ノート

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