Sodium Carbonate → 4,5-Dimethylpyridin-2-amine

HRID 869889ノート

反応式

HRID 869889 の反応式
[CH3:1][C:2]1[C:7]([CH3:8])=[CH:6][N:5]=[C:4]([N:9]2C(=O)C3C=CC=CC=3OC2(C)C)[CH:3]=1.C([O-])([O-])=O.[Na+].[Na+]>Cl>[CH3:1][C:2]1[C:7]([CH3:8])=[CH:6][N:5]=[C:4]([NH2:9])[CH:3]=1

参加物

4

反応物 2

HCID 10340Sodium CarbonateHCID 687366023-(4,5-Dimethylpyridin-2-yl)-2,2-dimethyl-2h-benzo[e][1,3]oxazin-4(3h)-one

生成物 1

HCID 124040134,5-Dimethylpyridin-2-amine収率 103.7%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

A solution of 3-(4,5-dimethylpyridin-2-yl)-2,2-dimethyl-2H-benzo[e][1,3]oxazin-4(3H)-one (9 g, 0.03 mol) in concentrated hydrochloric acid (100 mL) was heated at reflux overnight. The mixture was basified by saturated solution of Na2CO3 and extracted with CH2Cl2 (100 mL×3). The combined organic layers were dried over anhydrous Na2SO4, filtered and evaporated under vacuum to give 4,5-dimethylpyridin-2-amine (3.8 g, 97%), that was directly used in the next step without further purification.

後処理

  1. temperatureat reflux overnight
  2. extractionextracted with CH2Cl2 (100 mL×3)
  3. dry with materialThe combined organic layers were dried over anhydrous Na2SO4
  4. filtrationfiltered
  5. customevaporated under vacuum

出典と根拠

ORDレコード
ord-98f05b2c33c34d7d99ffa5c83fa8657f
出典データセット
uspto-grants-2015_03
特許番号
US08969386B2

反応ノート

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