2-Chloroethanol → 2-(2-Nitrophenoxy)ethanol
반응식
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[OH:10])([O-:3])=[O:2].[OH-].[Na+].O.Cl[CH2:15][CH2:16][OH:17]>C(O)CCC>[OH:17][CH2:16][CH2:15][O:10][C:5]1[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=1[N+:1]([O-:3])=[O:2]참가 물질
6
반응 조건
- 온도
- 100 °C
실험 절차
10 g (71.88 mmol) 2-nitrophenol A1 and 3.59 g (89.86 mmol) sodium hydroxide were dissolved in 55 ml n-butanol and 5 ml water at 70° C., 6.26 ml (7.52 g, 93.44 mmol) 2-chloroethanol were slowly added drop by drop. This was followed by three days of vigorous stirring at 100° C. After cooling, the reaction mixture was filtrated, the precipitate washed with chloroform and the filtrate reduced. The residue was taken up in chloroform and washed three times with aqueous 10% sodium hydroxide solution. Then the organic phase was dried over sodium sulfate and was concentrated in vacuo. 10.8 g of bright yellow crystals were obtained; yield 82%.
후처리
- customat 70° C.
- temperatureAfter cooling
- filtrationthe reaction mixture was filtrated
- washthe precipitate washed with chloroform
- washwashed three times with aqueous 10% sodium hydroxide solution
- dry with materialThen the organic phase was dried over sodium sulfate
- concentrationwas concentrated in vacuo
출처 및 근거
- ORD 기록
- ord-803d766689644a11b4247240b6f5a848
- 출처 데이터셋
- uspto-grants-1999_12
- 특허 번호
- US06001999
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