Lithium hydroxide, monohydrate → HCID 59333911、化合物
反応式
[F:1][C:2]([F:17])([F:16])[CH2:3][CH2:4][N:5]1[CH2:10][CH2:9][CH:8]([C:11]([O:13]CC)=[O:12])[CH2:7][CH2:6]1.O[Li].O>C1COCC1.CO>[F:17][C:2]([F:1])([F:16])[CH2:3][CH2:4][N:5]1[CH2:10][CH2:9][CH:8]([C:11]([OH:13])=[O:12])[CH2:7][CH2:6]1参加物
5
実験手順
To a solution of ethyl 1-(3,3,3-trifluoropropyl)piperidine-4-carboxylate (3.30 g, 13.0 mmol) in THF (40 mL) and MeOH (40 mL) was added LiOH—H2O (1.64 g, 39.1 mmol). The reaction was allowed to stir for 15 h at which time the solution was filtered to remove undissolved solids and the filtrate concentrated. The resulting material was diluted with water (10 mL), made to pH 5 with HCl (conc), then concentrated in vacuo to yield a white solid (2.9 g, 150%). Mass Spectrum: Calcd for C9H15NF3O2(M+H): 226. Found: 226.
後処理
- filtrationwas filtered
- customto remove undissolved solids
- concentrationthe filtrate concentrated
- additionThe resulting material was diluted with water (10 mL)
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-882523cf96a74efca644d7a5db9aa116
- 出典データセット
- uspto-grants-2012_05
- 特許番号
- US08183255B2
反応ノート
読み込み中…