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Methyl iodide → 2-Chloro-3-methoxypyridine

HRID 1037305
ノート
印刷プレビュー

反応式

HRID 1037305 の反応式
[Cl:1][C:2]1[C:7]([OH:8])=[CH:6][CH:5]=[CH:4][N:3]=1.[CH3:9][O-].[Na+].IC>CN(C=O)C>[Cl:1][C:2]1[C:7]([O:8][CH3:9])=[CH:6][CH:5]=[CH:4][N:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 811362-Chloro-3-pyridinolHCID 10942334Sodium Methoxide

生成物 1

HCID 1042522-Chloro-3-methoxypyridine収率 79%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a stirred solution of 2-chloro-3-hydroxypyridine (25.4 g, 196 mmol) in dry DMF (250 mL), at 0° C., was added sodium methoxide (11.5 g, 213 mmol). After 5 min, the reaction mixture was allowed to warm to RT. After 1 hour, the mixture was cooled to 0° C. and iodomethane (24 mL, 386 mmol) was added. The reaction mixture was stirred at 0° C. for 5 minutes, before allowing to warm to RT. After 2 hours, the reaction mixture was concentrated under reduced pressure. The resultant residue was partitioned between diethyl ether and water. The aqueous phase was isolated and extracted twice with diethyl ether. The combined organic extracts were washed with water, brine, dried (Na2SO4), filtered and concentrated in vacuo to give the title compound (22.2 g, 79%) as an orange solid. LCMS (Method A): RT=2.76 min, [M+H]+=144/146.

後処理

  1. waitAfter 1 hour
  2. temperaturethe mixture was cooled to 0° C.
  3. temperatureto warm to RT
  4. waitAfter 2 hours
  5. concentrationthe reaction mixture was concentrated under reduced pressure
  6. customThe resultant residue was partitioned between diethyl ether and water
  7. customThe aqueous phase was isolated
  8. extractionextracted twice with diethyl ether
  9. washThe combined organic extracts were washed with water, brine
  10. dry with materialdried (Na2SO4)
  11. filtrationfiltered
  12. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-c08ab2ebc3404938a14ddafb0f6dc8c4
出典データセット
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08546376B2

反応ノート

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