Hydrochloric Acid → HCID 86666036、化合物

HRID 469714

反応式

HRID 469714 の反応式
[C:1]([C:5]1[N:6]=[C:7]([NH:10][C:11]([C@@H:13]2[CH2:17][CH2:16][CH2:15][NH:14]2)=[O:12])[S:8][CH:9]=1)([CH3:4])([CH3:3])[CH3:2].Cl.C(N(CC)C(C)C)(C)C.[Cl:28][C:29]1[C:30](F)=[N:31][CH:32]=[C:33]([C:35]([F:38])([F:37])[F:36])[CH:34]=1>CS(C)=O>[C:1]([C:5]1[N:6]=[C:7]([NH:10][C:11]([C@@H:13]2[CH2:17][CH2:16][CH2:15][N:14]2[C:30]2[C:29]([Cl:28])=[CH:34][C:33]([C:35]([F:38])([F:36])[F:37])=[CH:32][N:31]=2)=[O:12])[S:8][CH:9]=1)([CH3:4])([CH3:2])[CH3:3]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 81531DiisopropylethylamineHCID 12680753-Chloro-2-fluoro-5-(trifluoromethyl)pyridineHCID 54959952(S)-pyrrolidine-2-carboxylic acid (4-tert-butyl-thiazol-2-yl)-amide

生成物 1

HCID 86666036HCID 86666036、化合物

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

反応条件

温度
100 °C

実験手順

To a vial containing (S)-pyrrolidine-2-carboxylic acid (4-tert-butyl-thiazol-2-yl)-amide; hydrochloride (0.212 g; 0.731 mmol) in dimethylsulfoxide (2 mL) is added N,N-diisopropylethylamine (0.127 mL; 0.731 mmol) and 3-chloro-2-fluoro-5-trifluoromethylpyridine (0.096 mL; 0.731 mmol). The mixture is heated at 100° C. for 1 hour in an oil bath and then cooled to room temperature. The crude mixture is filtered and purified by preparative HPLC chromatography. Product fractions are pooled and concentrated in vacuo to afford title compound. ESI m/z 433 [M+H]+

後処理

  1. temperaturecooled to room temperature
  2. filtrationThe crude mixture is filtered
  3. custompurified by preparative HPLC chromatography
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-8bcb9c11fc4f4614bdb451cb936af102
出典データセット
uspto-grants-2014_01
特許番号
US08629157B2

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