Water → 5,5-dimethyl-4H,5H,6H-cyclopenta[b]thiophene-2-carboxylic acid
반응식
[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]1참가 물질
6
반응 조건
- 온도
- 65 °C
실험 절차
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
후처리
- customThe organic solvents were removed under reduced pressure
- filtrationThe precipitate was collected by filtration
- customdried in vacuo
출처 및 근거
- ORD 기록
- ord-96f8f217f66146f28ef388f7c6fa3870
- 출처 데이터셋
- uspto-grants-2015_08
- 특허 번호
- US09115152B2
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