Sodium hydride → HCID 57878591、化合物
反応式
Cl[CH2:2][CH2:3][CH2:4][C:5]([NH:7][CH:8]1[CH2:13][CH2:12][C:11]([F:15])([F:14])[CH2:10][CH2:9]1)=[O:6].[H-].[Na+]>C1COCC1.CCOCC>[F:14][C:11]1([F:15])[CH2:12][CH2:13][CH:8]([N:7]2[CH2:2][CH2:3][CH2:4][C:5]2=[O:6])[CH2:9][CH2:10]1参加物
5
実験手順
Heat the mixture of 4-chloro-N-(4,4-difluoro-cyclohexyl)-butyramide (0.41 g, 1.7 mmol) and 0.69 g of NaH in 17 mL of THF to 70° C. for overnight. Dilute the reaction mixture with Et2O. Filter the precipitate through a pad of celite. Wash the organic layer with saturated aqueous NaCl, dry over Na2SO4, filter and concentrate. Purify the crude material by chromatography to afford 0.19 g of the title compound: mass spectrum (m/z): 204 (M+1).
後処理
- temperatureHeat
- filtrationFilter the precipitate through a pad of celite
- washWash the organic layer with saturated aqueous NaCl
- dry with materialdry over Na2SO4
- filtrationfilter
- concentrationconcentrate
- customPurify the crude material by chromatography
出典と根拠
- ORDレコード
- ord-13f9f43141344101b2d011c323a997b5
- 出典データセット
- uspto-grants-2011_08
- 特許番号
- US07998999B2
反応ノート
読み込み中…