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Acetic Acid → HCID 84071046, 화합물

HRID 1527095
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HRID 1527095 반응식
Cl[C:2]1[N:9]=[C:8]([CH3:10])[CH:7]=[C:6](Cl)[C:3]=1[C:4]#[N:5].[CH3:12][O-:13].[Na+].C[C:16]([OH:18])=O>CO>[CH3:12][O:13][C:2]1[N:9]=[C:8]([CH3:10])[CH:7]=[C:6]([O:18][CH3:16])[C:3]=1[C:4]#[N:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 10942334Sodium MethoxideHCID 112754712,4-Dichloro-6-methylnicotinonitrile

생성물 1

HCID 84071046HCID 84071046, 화합물수율 95%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

2,4-dichloro-6-methylnicotinonitrile (45 g, 240 mmol) was dissolved in CH3OH (300 ml). NaOMe (30% in MeOH, 100 ml, 1680 mmol) was added. The mixture was refluxed for 4 h. After cooled to r.t., the reaction mixture was neutralized by HOAc. The solvent was removed under vacuum and the residue was washed with H2O (300 ml) and MTBE (100 ml). The resulting solid was coevaporated with dry THF (300 ml) to give 2,4-dimethoxy-6-methylnicotinonitrile as a dark-yellow solid. (40 g, yield 95%).

후처리

  1. temperatureThe mixture was refluxed for 4 h
  2. customThe solvent was removed under vacuum
  3. washthe residue was washed with H2O (300 ml) and MTBE (100 ml)

출처 및 근거

ORD 기록
ord-0de657b547764411ad8dc0c6bbb09a7a
출처 데이터셋
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09085583B2

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