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

HRID 869889노트

반응식

HRID 869889 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 124040134,5-Dimethylpyridin-2-amine수율 103.7%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-98f05b2c33c34d7d99ffa5c83fa8657f
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08969386B2

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