Bromine → Ethyl 3-(2-amino-5-bromopyridin-4-yloxy)-4-chlorobenzoate

HRID 911035ノート

反応式

HRID 911035 の反応式
[NH2:1][C:2]1[CH:7]=[C:6]([O:8][C:9]2[CH:10]=[C:11]([CH:17]=[CH:18][C:19]=2[Cl:20])[C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH:5]=[CH:4][N:3]=1.[Br:21]Br>C(O)(=O)C>[NH2:1][C:2]1[CH:7]=[C:6]([O:8][C:9]2[CH:10]=[C:11]([CH:17]=[CH:18][C:19]=2[Cl:20])[C:12]([O:14][CH2:15][CH3:16])=[O:13])[C:5]([Br:21])=[CH:4][N:3]=1

参加物

4

反応物 2

HCID 24408BromineHCID 66617829Ethyl 3-(2-aminopyridin-4-yloxy)-4-chlorobenzoate

生成物 1

HCID 66617810Ethyl 3-(2-amino-5-bromopyridin-4-yloxy)-4-chlorobenzoate収率 61.4%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A flask was charged with ethyl 3-(2-aminopyridin-4-yloxy)-4-chlorobenzoate (5.50 g, 18.8 mmol) and acetic acid (50 mL), and bromine (0.943 ml, 18.4 mmol) was added. The reaction was stirred at ambient temperature for 30 minutes and then concentrated. The residue was purified by silica gel column chromatography, eluting with 20%-35% ethyl acetate in hexanes to give the desired product (4.20 g, 58.9% yield) as light yellow solid.

後処理

  1. additionwas added
  2. concentrationconcentrated
  3. customThe residue was purified by silica gel column chromatography
  4. washeluting with 20%-35% ethyl acetate in hexanes

出典と根拠

ORDレコード
ord-acb1015a38cd4fb2a8527bc7d186e04d
出典データセット
uspto-grants-2011_09
特許番号
US08022222B2

反応ノート

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