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Water → 4-[5-(3,5-Dichloro-phenyl)-5-trifluoromethyl-4,5-dihydro-isoxazol-3-yl]-2-methyl-benzaldehyde-4-trifluoroethylsemicarbazone

HRID 1525754
ノート
印刷プレビュー

反応式

HRID 1525754 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:9]2([C:23]([F:26])([F:25])[F:24])[O:13][N:12]=[C:11]([C:14]3[CH:21]=[CH:20][C:17]([CH:18]=O)=[C:16]([CH3:22])[CH:15]=3)[CH2:10]2)[CH:5]=[C:6]([Cl:8])[CH:7]=1.Cl.[F:28][C:29]([F:37])([F:36])[CH2:30][NH:31][C:32](=[O:35])[NH:33][NH2:34].O.CC(OC)(C)C>C(O)C.C(O)(=O)C>[F:28][C:29]([F:37])([F:36])[CH2:30][NH:31][C:32](=[O:35])[NH:33][N:34]=[CH:18][C:17]1[CH:20]=[CH:21][C:14]([C:11]2[CH2:10][C:9]([C:4]3[CH:3]=[C:2]([Cl:1])[CH:7]=[C:6]([Cl:8])[CH:5]=3)([C:23]([F:26])([F:24])[F:25])[O:13][N:12]=2)=[CH:15][C:16]=1[CH3:22]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 962WaterHCID 15413tert-Butyl methyl etherHCID 866585204-[5-(3,5-Dichloro-phenyl)-5-trifluoromethyl-4,5-dihydro-isoxazol-3-yl]-2-methyl-benzaldehydeHCID 86681562HCID 86681562、化合物

生成物 1

HCID 866815614-[5-(3,5-Dichloro-phenyl)-5-trifluoromethyl-4,5-dihydro-isoxazol-3-yl]-2-methyl-benzaldehyde-4-trifluoroethylsemicarbazone収率 86.3%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 702Ethanol溶媒

反応条件

温度
70 °C

実験手順

A mixture of 4-[5-(3,5-dichloro-phenyl)-5-trifluoromethyl-4,5-dihydro-isoxazol-3-yl]-2-methyl-benzaldehyde (72.5 g, 0.18 mol) and 4-trifluoroethyl semicarbazide hydrochloride (39.92 g, 0.21 mol) in ethanol (50 mL) and glacial acetic acid (40 mL) was heated at 70° C. over night. After this, water was added until the clear solution became turbid, then MTBE (10 mL) was added and the mixture was allowed to cool to ambient temperature. The resulting precipitate was filtered and washed with water to obtain the title compound (84.10 g, 86%).

後処理

  1. temperatureto cool to ambient temperature
  2. filtrationThe resulting precipitate was filtered
  3. washwashed with water

出典と根拠

ORDレコード
ord-ee3538c240d34ed9a6fe89785de81d1d
出典データセット
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09085541B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート