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

HRID 1891167노트

반응식

HRID 1891167 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-69edd3ebfa404ce68ec9bf4e4f6d1522
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08507480B2

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