Triethylamine → HCID 20407006、化合物

HRID 615537ノート

反応式

HRID 615537 の反応式
[CH3:1][C:2]([C:5]1[CH:9]=[C:8]([NH2:10])[O:7][N:6]=1)([CH3:4])[CH3:3].C(N(CC)CC)C.[CH3:18][CH:19]([CH2:23][CH2:24][Cl:25])[C:20](Cl)=[O:21]>C(OCC)(=O)C>[Cl:25][CH2:24][CH2:23][CH:19]([CH3:18])[C:20]([NH:10][C:8]1[O:7][N:6]=[C:5]([C:2]([CH3:4])([CH3:3])[CH3:1])[CH:9]=1)=[O:21]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 20956943-Tert-butyl-1,2-oxazol-5-amineHCID 137705824-Chloro-2-methylbutanoyl chloride

生成物 1

HCID 20407006HCID 20407006、化合物

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

To a stirred solution of 7 g of 3-(1,1-dimethylethyl)-5-aminoisoxazole dissolved in 50 ml ethyl acetate was added 5.05 g of triethylamine at room temperature. As the solution continued to stir, 8 g of 2-methyl-4-chlorobutyric acid chloride was added to the reaction mixture over a 15 minute period. The reaction was allowed to stir for about 3 days and the precipitated triethylamine hydrochloride salt was collected by filtration and washed with ethyl acetate. The solvent was evaporated from the filtrate under reduced pressure and the residue was recrystallized from diethyl ether to afford 4-chloro-N-[3-(1,1-dimethylethyl)-5-isoxazolyl]-2-methylbutanamide as a solid. mp 135°-137° C.

後処理

  1. stirringto stir for about 3 days
  2. filtrationthe precipitated triethylamine hydrochloride salt was collected by filtration
  3. washwashed with ethyl acetate
  4. customThe solvent was evaporated from the filtrate under reduced pressure
  5. customthe residue was recrystallized from diethyl ether

出典と根拠

ORDレコード
ord-148b9ed18c734c2f92180adc2ac95b53
出典データセット
uspto-grants-1985_02
特許番号
US04500343

反応ノート

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