Water → 5-(2,4-Bis-benzyloxy-5-bromo-phenyl)-isoxazole-3-carboxylic acid ethyl ester

HRID 1891156ノート

反応式

HRID 1891156 の反応式
[CH2:1]([O:3][C:4](=[O:33])[C:5](=O)[CH2:6][C:7]([C:9]1[CH:14]=[C:13]([Br:15])[C:12]([O:16][CH2:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)=[CH:11][C:10]=1[O:24][CH2:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)=[O:8])[CH3:2].Cl.[NH2:35]O.O>C(O)C>[CH2:1]([O:3][C:4]([C:5]1[CH:6]=[C:7]([C:9]2[CH:14]=[C:13]([Br:15])[C:12]([O:16][CH2:17][C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)=[CH:11][C:10]=2[O:24][CH2:25][C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[O:8][N:35]=1)=[O:33])[CH3:2]

参加物

5

反応物 3

HCID 962WaterHCID 443297Hydroxyamine hydrochlorideHCID 592648154-(2,4-Bis-benzyloxy-5-bromo-phenyl)-2,4-dioxo-butyric acid ethyl ester

生成物 1

HCID 247745225-(2,4-Bis-benzyloxy-5-bromo-phenyl)-isoxazole-3-carboxylic acid ethyl ester

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

69.3 g of 4-(2,4-Bis-benzyloxy-5-bromo-phenyl)-2,4-dioxo-butyric acid ethyl ester (0.135 mol, 1 eq) were dissolved in 750 ml ethanol. 14.11 g hydroxylamine hydrochloride (0.203 mol, 1.5 eq) were added. The mixture was refluxed for 2.5 hours and cooled down. It was then poured onto 1000 ml water, the precipitate was filtered off. The filter cake was washed with 500 ml of water followed by 75 ml diethyl ether and dried.

後処理

  1. temperatureThe mixture was refluxed for 2.5 hours
  2. temperaturecooled down
  3. filtrationthe precipitate was filtered off
  4. washThe filter cake was washed with 500 ml of water
  5. customdried

出典と根拠

ORDレコード
ord-645dab47333e4f09a67f64c674236be6
出典データセット
uspto-grants-2013_08
特許番号
US08507480B2

反応ノート

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