Acetic Anhydride → (4-Methylpyridin-2-yl)methyl acetate

반응식

[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][N+:3]=1[O-].[C:10]([O:13]C(=O)C)(=[O:12])[CH3:11]>>[CH3:8][C:6]1[CH:5]=[CH:4][N:3]=[C:2]([CH2:1][O:13][C:10](=[O:12])[CH3:11])[CH:7]=1

참가 물질

반응물 2

HCID 7918Acetic Anhydride

HCID 707332,4-Dimethylpyridine 1-oxide

생성물 1

HCID 19912996(4-Methylpyridin-2-yl)methyl acetate수율 29.8%

반응 조건

온도: 110 °C

실험 절차

Acetic anhydride (30 mL) was added to 2,4-dimethyl-pyridine 1-oxide (1.93 g, 15.7 mmol) described in Manufacturing Example 11-1-1, and the mixture was stirred for 10 minutes at 110° C. The reaction solution was allowed to room temperature and concentrated under a reduced pressure. The resulting residue was purified by silica gel column chromatography (heptane:ethyl acetate=1:2, then ethyl acetate) to obtain the title compound (774 mg, 29.8%).

후처리

customwas allowed to room temperature
concentrationconcentrated under a reduced pressure
customThe resulting residue was purified by silica gel column chromatography (heptane

출처 및 근거

ORD 기록: ord-7dc5a4e539194560a9d0bd0764d574e8
출처 데이터셋: uspto-grants-2010_04
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US07691882B2

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