Lithium Hydroxide → 2-Amino-4,6-diisopropoxy-nicotinic acid

HRID 591783ノート

反応式

HRID 591783 の反応式
C[O:2][C:3](=[O:19])[C:4]1[C:9]([O:10][CH:11]([CH3:13])[CH3:12])=[CH:8][C:7]([O:14][CH:15]([CH3:17])[CH3:16])=[N:6][C:5]=1[NH2:18].[OH-].[Li+]>CO.O>[NH2:18][C:5]1[N:6]=[C:7]([O:14][CH:15]([CH3:16])[CH3:17])[CH:8]=[C:9]([O:10][CH:11]([CH3:13])[CH3:12])[C:4]=1[C:3]([OH:19])=[O:2]

参加物

5

反応物 2

HCID 3939Lithium HydroxideHCID 666709872-Amino-4,6-diisopropoxy-nicotinic acid methyl ester

生成物 1

HCID 666710672-Amino-4,6-diisopropoxy-nicotinic acid

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

反応条件

温度
50 °C

実験手順

To the solution of 2-amino-4,6-diisopropoxy-nicotinic acid methyl ester (1.6 g, 5.97 mmol) in methanol (9.0 mL) and water (1.0 mL), was added lithium hydroxide (750 mg, 17.91 mmol). The reaction mixture was heated to 50° C. for 8 hours. The solvent was removed; the residue was diluted with water and neutralized with 2 N HCl. The product was extracted with ethyl acetate (3×100 mL). The combined organic layer was washed with water, then brine, dried over Na2SO4, and evaporated, to give crude 2-amino-4,6-diisopropoxy-nicotinic acid as a light yellow solid. Yield: 1.48 g (98%, crude).

後処理

  1. customThe solvent was removed
  2. additionthe residue was diluted with water and neutralized with 2 N HCl
  3. extractionThe product was extracted with ethyl acetate (3×100 mL)
  4. washThe combined organic layer was washed with water
  5. dry with materialbrine, dried over Na2SO4
  6. customevaporated

出典と根拠

ORDレコード
ord-ada7c9549a194c1ba89326a121c6f78b
出典データセット
uspto-grants-2016_01
特許番号
US09238640B2

反応ノート

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