Chloroform → Methyl 3-chloromethylpyrazine-2-carboxylate

HRID 604817노트

반응식

HRID 604817 반응식
[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

참가 물질

4

반응물 3

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

생성물 1

HCID 67039637Methyl 3-chloromethylpyrazine-2-carboxylate수율 52%

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a785675770ee45caa7784f4fe24d4d9b
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07910735B2

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