2-Aminothiophenol → 1-(2-Benzothiazol-2-ylmethylpiperidin-1-yl)-2,2,2-trifluoroethanone

HRID 2377995노트

반응식

HRID 2377995 반응식
C(O[C:4](=O)[CH2:5][CH:6]1[CH2:11][CH2:10][CH2:9][CH2:8][N:7]1[C:12](=[O:17])[C:13]([F:16])([F:15])[F:14])C.[NH2:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=1[SH:26]>O>[S:26]1[C:21]2[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=2[N:19]=[C:4]1[CH2:5][CH:6]1[CH2:11][CH2:10][CH2:9][CH2:8][N:7]1[C:12](=[O:17])[C:13]([F:14])([F:15])[F:16]

참가 물질

4

반응물 2

HCID 87132-AminothiophenolHCID 86625769[1-(2,2,2-Trifluoroethanoyl)piperidin-2-yl] acetic acid ethyl ester

생성물 1

HCID 231464011-(2-Benzothiazol-2-ylmethylpiperidin-1-yl)-2,2,2-trifluoroethanone

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
90 °C

실험 절차

[1-(2,2,2-Trifluoroethanoyl)piperidin-2-yl] acetic acid ethyl ester, D28 (1.34 g) and 2-aminothiophenol (1.50 g) were suspended in polyphosphoric acid (30 ml) and heated to 90° C. for 2 h with vigorous stirring. After cooling, the reaction mixture was poured into iced water and stirred vigorously for 1 h. The aqueous solution was then extracted several times with ethyl acetate. After drying (MgSO4), the solvent was removed in vacuo and the residue chromatographed (silica gel) to afford the title compound as an oil (1.2 g).

후처리

  1. temperatureAfter cooling
  2. extractionThe aqueous solution was then extracted several times with ethyl acetate
  3. dry with materialAfter drying (MgSO4)
  4. customthe solvent was removed in vacuo
  5. customthe residue chromatographed (silica gel)

출처 및 근거

ORD 기록
ord-fe0a6c6294504a7884ec0b76fec06e72
출처 데이터셋
uspto-grants-2008_12
특허 번호
US07470710B2

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