Methanol → 3-Amino-2-methylbenzoic acid methyl ester

HRID 2208723ノート

反応式

HRID 2208723 の反応式
C[C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[C:4]([CH3:11])[C:3]=1[NH2:12].OS(O)(=O)=O.[CH3:18]O>>[NH2:12][C:3]1[C:4]([CH3:11])=[C:5]([CH:9]=[CH:10][CH:2]=1)[C:6]([O:8][CH3:18])=[O:7]

参加物

4

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 22754770HCID 22754770、化合物

生成物 1

HCID 38010253-Amino-2-methylbenzoic acid methyl ester収率 91%

反応条件

温度
70 °C

実験手順

To stirred solution of methyl 3-amino-2-methylbenzoic acid (5 g, 33.1 mmol) in methanol (50 mL), was added conc. H2SO4 (5 mL) at 0° C. and the mixture was heated at 70° C. for 22 h. On completion, methanol was removed under reduced pressure, and then sat. sodium bicarbonate solution was added and the product extracted with 10% MeOH/DCM. Combined organic layers were dried, concentrated to yield methyl 3-amino-2-methylbenzoate (5 g, 91%).

後処理

  1. customOn completion, methanol was removed under reduced pressure
  2. additionsat. sodium bicarbonate solution was added
  3. extractionthe product extracted with 10% MeOH/DCM
  4. customCombined organic layers were dried
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-6255ec5fb7dc493c926ee410e2ec2e5c
出典データセット
uspto-grants-2016_06
特許番号
US09376422B2

反応ノート

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