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

HRID 2377995ノート

反応式

HRID 2377995 の反応式
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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
90 °C

実験手順

[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).

後処理

  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)

出典と根拠

ORDレコード
ord-fe0a6c6294504a7884ec0b76fec06e72
出典データセット
uspto-grants-2008_12
特許番号
US07470710B2

反応ノート

読み込み中…