Trifluoroacetic acid → 2-Methyl-1-(piperazin-1-yl)propan-2-ol
反応式
[OH:1][C:2]([CH3:18])([CH3:17])[CH2:3][N:4]1[CH2:9][CH2:8][N:7](C(OCCCC)=O)[CH2:6][CH2:5]1.C(O)(C(F)(F)F)=O>C(Cl)Cl>[CH3:18][C:2]([OH:1])([CH3:17])[CH2:3][N:4]1[CH2:5][CH2:6][NH:7][CH2:8][CH2:9]1参加物
4
実験手順
A solution of 563 (460 mg, 1.78 mmol) and TFA (5 ml) in DCM (20 ml) was stirred at rt for 5 h. The reaction mixture was concentrated (azeotropes with DCM), diluted with water, stirred for 10 min. The pH was adjusted to around 10 with 1N NaOH, and the alkaline solution was extracted with DCM. The organic extract was dried over anhydrous magnesium sulfate, filtered, concentrated under high vacuum to afford the desired product 564 (170 mg, 1.07 mmol, 60% yield) as a dark orange sticky solid. The crude product was used in the next step without any further purification. MS (m/z): 159.13 (M+H).
後処理
- concentrationThe reaction mixture was concentrated (azeotropes with DCM)
- additiondiluted with water
- extractionthe alkaline solution was extracted with DCM
- extractionThe organic extract
- dry with materialwas dried over anhydrous magnesium sulfate
- filtrationfiltered
- concentrationconcentrated under high vacuum
出典と根拠
- ORDレコード
- ord-7aedf231f96e4fe5ab6740cafd189957
- 出典データセット
- uspto-grants-2014_12
- 特許番号
- US08906852B2
反応ノート
読み込み中…