Water → 1,2-Benzenediethanol
반응식
[C:1]1([CH2:11][C:12](O)=[O:13])[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[CH2:7][C:8](O)=[O:9].[H-].[H-].[H-].[H-].[Li+].[Al+3].O.[OH-].[Na+]>C1COCC1>[C:2]1([CH2:7][CH2:8][OH:9])[CH:3]=[CH:4][CH:5]=[CH:6][C:1]=1[CH2:11][CH2:12][OH:13]참가 물질
6
실험 절차
To a solution of 2,2′-(1,2-phenylene)diacetic acid (10 g, 51.5 mmol) in THF (100 mL) was added to LAH in THF (90 mL) dropwise, the mixture was refluxed for 18 hours. The mixture was cooled in ice bath and carefully added water (8 mL) dropwise, followed by 1 N NaOH (8 mL), then removed the ice bath added water slowly with stirring until the gray precipitate turns white. The mixture was filtrated and the filtrate was concentrated to give crude 2,2′-(1,2-phenylene)diethanol (8 g, 94%). 1H-NMR (CDCl3): 2.02 (s, 3H), 2.97 (m, 4H), 3.83 (m, 2H), 4.12 (m, 1H), 4.24 (t, 1H), 7.19 (m, 4H).
후처리
- temperaturethe mixture was refluxed for 18 hours
- temperatureThe mixture was cooled in ice bath
- customremoved the ice bath
- additionadded water slowly
- filtrationThe mixture was filtrated
- concentrationthe filtrate was concentrated
출처 및 근거
- ORD 기록
- ord-0ec52081ca09468e8e2c417ed39c15a3
- 출처 데이터셋
- uspto-grants-2014_01
- 특허 번호
- US08633212B2
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