Methyl bromoacetate → [4-(3-Benzo[d]isoxazolylimino)-1-(4H)-pyridinyl]-acetic acid methyl ester hydrobromide

HRID 2149

反応式

HRID 2149 の反応式
[N:1]1[CH:6]=[CH:5][C:4]([NH:7][C:8]2[C:12]3[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=3[O:10][N:9]=2)=[CH:3][CH:2]=1.[Br:17][CH2:18][C:19]([O:21][CH3:22])=[O:20]>C(#N)C>[BrH:17].[CH3:22][O:21][C:19](=[O:20])[CH2:18][N:1]1[CH:2]=[CH:3][C:4](=[N:7][C:8]2[C:12]3[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=3[O:10][N:9]=2)[CH:5]=[CH:6]1

参加物

4

反応物 2

HCID 60984Methyl bromoacetateHCID 98372191,2-Benzisoxazol-3-amine, N-4-pyridinyl-

生成物 1

HCID 70280625[4-(3-Benzo[d]isoxazolylimino)-1-(4H)-pyridinyl]-acetic acid methyl ester hydrobromide収率 70%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A mixture of 3-(4-pyridinylamino)-1,2-benzisoxazole (0.9 g, 4.3 mmol) and methyl bromoacetate (0.44 mL, 1.1 eq) in acetonitrile (25 mL) was heated at reflux for one hour. The mixture was then allowed to cool to room temperature and the precipitated product was collected by filtration. The white solid was washed with diethyl ether and dried under vacuum to provide the title compound (1.1 g, 70%), mp 235-236° C.

後処理

  1. temperaturewas heated
  2. temperatureat reflux for one hour
  3. filtrationthe precipitated product was collected by filtration
  4. washThe white solid was washed with diethyl ether
  5. customdried under vacuum

出典と根拠

ORDレコード
ord-dc610c599a6a47cbbab5dcc6ac8c553a
出典データセット
uspto-grants-1998_03
特許番号
US05728717

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