1,2-Dichloroethane → Ethyl 3-aminopyridine-2-carboxylate

HRID 550362

反応式

HRID 550362 の反応式
[NH2:1][C:2]1[C:3]([C:8]([OH:10])=[O:9])=[N:4][CH:5]=[CH:6][CH:7]=1.[CH2:11](Cl)[CH2:12]Cl>C(O)C.CN(C1C=CN=CC=1)C>[NH2:1][C:2]1[C:3]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[N:4][CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 2

HCID 111,2-DichloroethaneHCID 738363-Aminopicolinic acid

生成物 1

HCID 565054Ethyl 3-aminopyridine-2-carboxylate収率 130.5%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒2 回HCID 702Ethanol溶媒

実験手順

3-Amino-2-picolinic acid (4.14 g) was suspended in ethanol (100 ml) at room temperature with stirring. DMAP (3.7 g) was added and the reaction was stirred for 1 hour at room temperature. A further equivalent of DMAP (3.7 g) was added and the suspension disappeared, and then EDC (5.80 g) was added and the reaction was stirred at room temperature for 17 hours. The ethanol was evaporated to give a dark oil, water was added and the mixture was extracted with ethyl acetate, washed with brine and dried over magnesium sulphate. Evaporation of the solvent gave ethyl 3-amino-2-picolinate as a solid (6.5 g), mixed in a 2:1 ratio with DMAP.

後処理

  1. stirringthe reaction was stirred for 1 hour at room temperature
  2. stirringthe reaction was stirred at room temperature for 17 hours
  3. customThe ethanol was evaporated
  4. customto give a dark oil, water
  5. additionwas added
  6. extractionthe mixture was extracted with ethyl acetate
  7. washwashed with brine
  8. dry with materialdried over magnesium sulphate
  9. customEvaporation of the solvent

出典と根拠

ORDレコード
ord-05ebb534ff354b0da15d4370faf4a9a9
出典データセット
uspto-grants-2011_05
特許番号
US07947679B2

関連ノート

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