Water → HCID 22768144、化合物

HRID 461362ノート

反応式

HRID 461362 の反応式
[C:1]([C:5]1[O:9][N:8]=[C:7]([NH:10][C:11](=[O:14])[O:12][CH3:13])[CH:6]=1)([CH3:4])([CH3:3])[CH3:2].C([O-])(=O)C.[Na+].[Br:20]Br.O>C(O)(=O)C.C(O)=O.C(Cl)Cl>[Br:20][C:6]1[C:7]([NH:10][C:11](=[O:14])[O:12][CH3:13])=[N:8][O:9][C:5]=1[C:1]([CH3:4])([CH3:2])[CH3:3]

参加物

8

反応物 4

HCID 962WaterHCID 24408Bromine2 回HCID 517045Sodium Acetate2 回HCID 13309592Carboxazole

生成物 1

HCID 22768144HCID 22768144、化合物収率 99.1%

試薬・触媒・溶媒 3

HCID 284Formic Acid触媒HCID 176Acetic Acid溶媒2 回HCID 6344Dichloromethane溶媒

反応条件

温度
70 °C

実験手順

To a solution of methyl 5-t-butyl-3-isoxazolylcarbamate (2.00 g) and anhydrous sodium acetate (1.1 mol equivalent) in glacial acetic acid (5 ml), bromine (1.0 mol equivalent) is added. The resultant mixture is heated at 50° C for 53 hours and mixed with glacial acetic acid (5 ml), anhydrous sodium acetate (0.91 g) and bromine (0.81 g). The mixture is heated at 70° C for 31 hours, mixed with several drops of formic acid, poured onto icy water (50 ml) and shaken with methylene chloride. The organic layer is washed with a saturated aqueous solution of sodium bicarbonate and water in order and evaporated under reduced pressure to remove the solvent, whereby methyl 4-bromo-5-t-butyl-3-isoxazolylcarbamate(2.77 g) is obtained as an oil. I.R.: 1774, 1203 cm-1 (CCl4).

後処理

  1. washThe organic layer is washed with a saturated aqueous solution of sodium bicarbonate and water in order
  2. customevaporated under reduced pressure
  3. customto remove the solvent

出典と根拠

ORDレコード
ord-d0282f47220340879e94fc6f65c76ad8
出典データセット
uspto-grants-1977_12
特許番号
US04062861

反応ノート

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