Hydrochloric Acid → HCID 86666036, 화합물

HRID 469714

반응식

HRID 469714 반응식
[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]

참가 물질

6

반응물 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

생성물 1

HCID 86666036HCID 86666036, 화합물

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

반응 조건

온도
100 °C

실험 절차

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]+

후처리

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

출처 및 근거

ORD 기록
ord-8bcb9c11fc4f4614bdb451cb936af102
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08629157B2

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