Hydrochloric Acid → HCID 67458346, 화합물

HRID 469709

반응식

HRID 469709 반응식
[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]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 12680753-Chloro-2-fluoro-5-(trifluoromethyl)pyridineHCID 67455816HCID 67455816, 화합물

생성물 1

HCID 67458346HCID 67458346, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
175 °C

실험 절차

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]+.

후처리

  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

출처 및 근거

ORD 기록
ord-7db17c660c714c0eab8397d3ea7c2c51
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08629157B2

연결된 노트

불러오는 중…