Sodium hydride → 4-Methoxy-2-(3-methyl-1,2,4-oxadiazol-5-yl)benzenamine

HRID 53244

反応式

HRID 53244 の反応式
[H-].[Na+].[C:3](=[N:6][OH:7])([NH2:5])[CH3:4].[NH2:8][C:9]1[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[CH:15][C:10]=1[C:11](OC)=O>O1CCCC1>[CH3:20][O:19][C:16]1[CH:17]=[CH:18][C:9]([NH2:8])=[C:10]([C:11]2[O:7][N:6]=[C:3]([CH3:4])[N:5]=2)[CH:15]=1

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 30926N-HydroxyacetamidineHCID 13052275Methyl 2-amino-5-methoxybenzoate

生成物 1

HCID 199621234-Methoxy-2-(3-methyl-1,2,4-oxadiazol-5-yl)benzenamine収率 72.4%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

Sodium hydride (594 mg) was added to a stirred suspension of acetamide oxime (1.0 g) and 4 molecular sieves (4 g) in dry tetrahydrofuran (50 ml) under nitrogen. The mixture was heated at 60° for 30 min then allowed to cool to room temperature. A solution of 2-amino-5-methoxybenzoic acid, methyl ester (2.0 g) in dry tetrahydrofuran (20 ml) was added and the mixture stirred at reflux for 2.5 h. The suspension was allowed to cool, filtered and the filtrate evaporated to give the title compound as a yellow solid (1.64 g)

後処理

  1. temperatureThe mixture was heated at 60° for 30 min
  2. temperatureat reflux for 2.5 h
  3. temperatureto cool
  4. filtrationfiltered
  5. customthe filtrate evaporated

出典と根拠

ORDレコード
ord-de14df84f908491bba4e59f0038f2dee
出典データセット
uspto-grants-1997_04
特許番号
US05618827

関連ノート

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