Ethylamine → 5-(2,4-Bis-benzyloxy-5-tert-butyl-phenyl)-isoxazole-3-carboxylic acid ethylamide

HRID 646496ノート

反応式

HRID 646496 の反応式
C(O[C:4]([C:6]1[CH:10]=[C:9]([C:11]2[CH:16]=[C:15]([C:17]([CH3:20])([CH3:19])[CH3:18])[C:14]([O:21][CH2:22][C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)=[CH:13][C:12]=2[O:29][CH2:30][C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)[O:8][N:7]=1)=[O:5])C.[CH2:37]([NH2:39])[CH3:38]>CO>[CH2:37]([NH:39][C:4]([C:6]1[CH:10]=[C:9]([C:11]2[CH:16]=[C:15]([C:17]([CH3:19])([CH3:18])[CH3:20])[C:14]([O:21][CH2:22][C:23]3[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=3)=[CH:13][C:12]=2[O:29][CH2:30][C:31]2[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=2)[O:8][N:7]=1)=[O:5])[CH3:38]

参加物

4

反応物 2

HCID 6341EthylamineHCID 247738805-(2,4-Bis-benzyloxy-5-tert-butyl-phenyl)-isoxazole-3-carboxylic acid ethyl ester

生成物 1

HCID 247733555-(2,4-Bis-benzyloxy-5-tert-butyl-phenyl)-isoxazole-3-carboxylic acid ethylamide

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

5-(2,4-Bis-benzyloxy-5-tert-butyl-phenyl)-isoxazole-3-carboxylic acid ethyl ester (10.0 g, 20.6 mmol) was added to a solution of ethylamine in methanol (60 ml, 2.0M) and the suspension heated, oil bath temperature 75° C., for ˜2 hrs. The resulting solution was allowed to cool and concentrated to a pale brown oil, dichloromethane (150 ml) was added and the solution washed with water (100 ml) and saturated aqueous sodium chloride solution (75 ml). The solution was dried over anhydrous sodium sulphate and concentrated to a brown oil, solidified on standing (9.9 g, ˜quant).

後処理

  1. temperaturethe suspension heated
  2. temperatureto cool
  3. concentrationconcentrated to a pale brown oil, dichloromethane (150 ml)
  4. additionwas added
  5. washthe solution washed with water (100 ml) and saturated aqueous sodium chloride solution (75 ml)
  6. dry with materialThe solution was dried over anhydrous sodium sulphate
  7. concentrationconcentrated to a brown oil

出典と根拠

ORDレコード
ord-4d2c62cc8e86439e95a2b426d8d49638
出典データセット
uspto-grants-2010_04
特許番号
US07705027B2

反応ノート

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