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Hydrochloric Acid → 3-Methoxy-6-methylpyrazine-2-carbaldehyde

HRID 890054
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HRID 890054 반응식
[CH3:1][O:2][C:3]1[C:4]([C:10](OC)=[O:11])=[N:5][C:6]([CH3:9])=[CH:7][N:8]=1.[H-].C([Al+]CC(C)C)C(C)C.Cl>C1(C)C=CC=CC=1>[CH3:1][O:2][C:3]1[C:4]([CH:10]=[O:11])=[N:5][C:6]([CH3:9])=[CH:7][N:8]=1
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참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 21225700DiisobutylaluminumhydrideHCID 22247866Methyl 3-methoxy-6-methylpyrazine-2-carboxylate

생성물 1

HCID 222482793-Methoxy-6-methylpyrazine-2-carbaldehyde수율 47.1%

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
-78 °C

실험 절차

After dissolving 300 mg of methyl 3-methoxy-6-methylpyrazine-2-carboxylate in a mixture of 5 ml toluene/5 ml dichloromethane, the solution was cooled to −78° C. Next, 1.21 ml of diisobutylaluminium hydride (1.5 M, toluene solution) was added dropwise and the mixture was stirred for 1 hour. After adding 10 ml of 1N hydrochloric acid dropwise to the reaction solution, extraction was performed with ethyl acetate. The organic layer was washed with 1N hydrochloric acid, a saturated sodium bicarbonate solution and saturated brine in that order and dried over anhydrous magnesium sulfate, and then the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (solvent: n-hexane/ethyl acetate) to obtain the title compound (118 mg, 47% yield).

후처리

  1. extractiondropwise to the reaction solution, extraction
  2. washThe organic layer was washed with 1N hydrochloric acid
  3. dry with materiala saturated sodium bicarbonate solution and saturated brine in that order and dried over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (solvent: n-hexane/ethyl acetate)

출처 및 근거

ORD 기록
ord-4020ec24eac04aa3a84f3c35fa88ea06
출처 데이터셋
uspto-grants-2006_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06995144B2

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