반응식
[C:1]1(=O)[O:5][CH2:4][CH2:3][O:2]1.[I:7][C:8]1[CH:13]=[CH:12]C(O)=[CH:10][CH:9]=1.C(=O)([O-])[O-].[K+].[K+].Cl.[OH-].[Na+]>>[OH:5][CH2:4][CH2:3][O:2][C:1]1[CH:12]=[CH:13][C:8]([I:7])=[CH:9][CH:10]=1참가 물질
반응 조건
- 온도
- 90 °C
실험 절차
A melt of ethylene carbonate (6.5 g, 74 mmol) in a small flask under Argon was treated with 4-iodophenol (0.400 g, 1.82 mmol) and powdered potassium carbonate (1.26 g, 9.1 mmol) and was stirred at 90° C. for 3 hr. The mixture was treated with cold dilute hydrochloric acid to decompose the excess potassium carbonate and excess aqueous sodium hydroxide solution was slowly added and the mixture was stirred over night. The suspension was extracted with methylene chloride, was washed with water and brine, was dried over sodium sulfate and was stripped to afford a white solid, which was purified by flash chromatography on silica gel (20 mL) with methylene chloride to afford (0.128 g, 27%) of the titled intermediate as a white solid, mp 76°-77.5° C.
후처리
- additionwas slowly added
- stirringthe mixture was stirred over night
- extractionThe suspension was extracted with methylene chloride
- washwas washed with water and brine
- dry with materialwas dried over sodium sulfate
- customto afford a white solid, which
- customwas purified by flash chromatography on silica gel (20 mL) with methylene chloride
출처 및 근거
- ORD 기록
- ord-2b2efe22dbd0427d9cf24b213a8634f8
- 출처 데이터셋
- uspto-grants-1999_01
- 특허 번호
- US05861421
연결된 노트
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