Hydrochloric Acid → 1-(3-Chloro-5-trifluoromethyl-pyridin-2-yl)-pyrrolidine-2-carboxylic acid (5-tert-butyl-isoxazol-3-yl)-amide

HRID 469709

反応式

HRID 469709 の反応式
[C:1]([C:5]1[O:9][N:8]=[C:7]([NH:10][C:11]([C@@H:13]2[CH2:17][CH2:16][CH2:15][NH:14]2)=[O:12])[CH:6]=1)([CH3:4])([CH3:3])[CH3:2].Cl.[Cl:19][C:20]1[C:21](F)=[N:22][CH:23]=[C:24]([C:26]([F:29])([F:28])[F:27])[CH:25]=1.C(N(CC)CC)C>C(O)C>[C:1]([C:5]1[O:9][N:8]=[C:7]([NH:10][C:11]([CH:13]2[CH2:17][CH2:16][CH2:15][N:14]2[C:21]2[C:20]([Cl:19])=[CH:25][C:24]([C:26]([F:29])([F:27])[F:28])=[CH:23][N:22]=2)=[O:12])[CH:6]=1)([CH3:4])([CH3:2])[CH3:3]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 12680753-Chloro-2-fluoro-5-(trifluoromethyl)pyridineHCID 67455816HCID 67455816、化合物

生成物 1

HCID 674583461-(3-Chloro-5-trifluoromethyl-pyridin-2-yl)-pyrrolidine-2-carboxylic acid (5-tert-butyl-isoxazol-3-yl)-amide

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
175 °C

実験手順

A microwave reaction vessel is charged with (S)-pyrrolidine-2-carboxylic acid (5-tert-butyl-isoxazol-3-yl)-amide; hydrochloride, 3-chloro-2-fluoro-5-trifluoromethylpyridine, triethylamine and ethanol. The mixture is heated in a microwave reactor at 175° C. for 1 h, maintaining the watts at 60 to keep the reactor from shutting down. The reaction is cooled to room temperature and concentrated in vacuo to afford an oil which is purified by reverse phase preparative HPLC. Product fractions are combined and concentrated in vacuo to afford title compound (64.4 mg). ESI m/z 417 [M+H]+.

後処理

  1. customA microwave reaction vessel
  2. temperaturemaintaining the watts at 60
  3. temperatureThe reaction is cooled to room temperature
  4. concentrationconcentrated in vacuo
  5. customto afford an oil which
  6. customis purified by reverse phase preparative HPLC
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-7db17c660c714c0eab8397d3ea7c2c51
出典データセット
uspto-grants-2014_01
特許番号
US08629157B2

関連ノート

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