Potassium Carbonate → (R)-(1-Methyl-2,2,2-trifluoroethyl)-thiourea
反応式
C([NH:9][C:10]([NH:12][C@H:13]([CH3:18])[C:14]([F:17])([F:16])[F:15])=[S:11])(=O)C1C=CC=CC=1.C(=O)([O-])[O-].[K+].[K+]>CO.O>[CH3:18][C@@H:13]([NH:12][C:10]([NH2:9])=[S:11])[C:14]([F:17])([F:16])[F:15]参加物
5
実験手順
Dissolve (R)-1-benzoyl-3-(1-methyl-2,2,2-trifluoroethyl)-thiourea (6.2 g, 22.5 mmol) in methanol and add a solution of potassium carbonate (13.8 g, 100 mmol) in water (30 mL). Stir vigorously at room temperature overnight. Evaporate to dryness, dissolve residue in hot water (ca. 100 mL) and filter the resulting white crystals. Cool filtrate to 0° C., seed with crystals from hot water filtration, filter and collect resulting white crystals to obtain the desired intermediate (2.9 g, 74%). MS (ES+) m/z: 173 (M+H)+.
後処理
- customEvaporate to dryness
- dissolutiondissolve residue in hot water (ca. 100 mL)
- filtrationfilter the resulting white crystals
- filtrationCool filtrate to 0° C., seed with crystals from hot water filtration
- filtrationfilter
- customcollect
- customresulting white crystals
出典と根拠
- ORDレコード
- ord-c717b8cd54c340759867ca97ec07b607
- 出典データセット
- uspto-grants-2014_03
- 特許番号
- US08680091B2
反応ノート
読み込み中…