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

HRID 1891156노트

반응식

HRID 1891156 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-645dab47333e4f09a67f64c674236be6
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08507480B2

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