Sodium Hydroxide → 6-Methoxy-5-methylpyridin-2-amine

HRID 1772913ノート

反応式

HRID 1772913 の反応式
[OH-].[Na+].[CH3:3][O:4][C:5]1[N:10]=[C:9]([NH:11]C(=O)C)[CH:8]=[CH:7][C:6]=1[CH3:15]>CO.O>[CH3:3][O:4][C:5]1[N:10]=[C:9]([NH2:11])[CH:8]=[CH:7][C:6]=1[CH3:15]

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 90030978N-(6-methoxy-5-methylpyridin-2-yl)acetamide2 回

生成物 1

HCID 900221706-Methoxy-5-methylpyridin-2-amine収率 194.3%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

反応条件

温度
90 °C

実験手順

A 10% solution of aqueous NaOH (40 mL) was added to a solution of N-(6-methoxy-5-methylpyridin-2-yl)acetamide (2.21 g, 12.3 mmol) in MeOH (160 mL) and the reaction mixture was heated at 90° C. for 3 d. After cooling to rt and concentration in vacuo to remove the MeOH the aqueous residue was combined with that from a previous batch derived from N-(6-methoxy-5-methylpyridin-2-yl)acetamide (2.21 g, 12.3 mmol). The aqueous phase was diluted with H2O (40 mL) and extracted with DCM (3×150 mL). The combined organic phases were washed with brine, dried (Na2SO4) and combined with a previous batch of crude 6-methoxy-5-methylpyridin-2-amine (266 mg). Concentration in vacuo yielded the title compound (3.30 g, 23.9 mmol).

後処理

  1. temperatureAfter cooling to rt
  2. concentrationconcentration in vacuo
  3. customto remove the MeOH the aqueous residue
  4. extractionextracted with DCM (3×150 mL)
  5. washThe combined organic phases were washed with brine
  6. dry with materialdried (Na2SO4)
  7. concentrationConcentration in vacuo

出典と根拠

ORDレコード
ord-4a2b32b1f6ce4e7ca2ec7bd9a4bff329
出典データセット
uspto-grants-2016_02
特許番号
US09249160B2

反応ノート

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