Water → 5,5-dimethyl-4H,5H,6H-cyclopenta[b]thiophene-2-carboxylic acid
反応式
[CH3:1][C:2]1([CH3:15])[CH2:14][C:5]2[S:6][C:7]([C:9]([O:11]CC)=[O:10])=[CH:8][C:4]=2[CH2:3]1.O.[OH-].[Li+]>CC(O)C.O1CCCC1>[CH3:1][C:2]1([CH3:15])[CH2:14][C:5]2[S:6][C:7]([C:9]([OH:11])=[O:10])=[CH:8][C:4]=2[CH2:3]1参加物
6
反応条件
- 温度
- 65 °C
実験手順
To a solution of 131c (16.0 g, 71.0 mmol) in propan-2-ol (200 mL), tetrahydrofuran (200 mL), and water (200 mL) was added lithium hydroxide (6.82 g, 284 mmol). See FIG. 15. The reaction mixture was heated at 65° C. for 5 h. The organic solvents were removed under reduced pressure. The pH of the residue was adjusted to 1.0 with hydrochloride acid (12M). The precipitate was collected by filtration and dried in vacuo to afford 131d (12.0 g, 86%) as a white solid. MS-ESI: [M+H]+ 196.9
後処理
- customThe organic solvents were removed under reduced pressure
- filtrationThe precipitate was collected by filtration
- customdried in vacuo
出典と根拠
- ORDレコード
- ord-96f8f217f66146f28ef388f7c6fa3870
- 出典データセット
- uspto-grants-2015_08
- 特許番号
- US09115152B2
反応ノート
読み込み中…