반응식
[Cr](Cl)([O-])(=O)=O.[NH+]1C=CC=CC=1.[CH2:12]([O:19][CH2:20][CH2:21][CH2:22][CH2:23][OH:24])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>ClCCl>[CH2:12]([O:19][CH2:20][CH2:21][CH2:22][CH:23]=[O:24])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1참가 물질
4
실험 절차
36.6 g (170 mmol) of pyridinium chlorochromate are placed at room temperature in 120 ml of dichloromethane under N2, and a solution of 20.4 g (113 mmol) of 4-benzyloxybutanol in 20 ml of dichloromethane is added. The reaction mixture rapidly becomes dark and the reaction is slightly exothermic. The reaction mixture is stirred at room temperature for 31/2 hours. The supernatant dichloromethane phase is decanted off and concentrated by evaporation in a rotary evaporator. The residue is filtered over 100 g of silica gel. The product fractions are concentrated by evaporation in a rotary evaporator and distilled under a high vacuum over a 10 cm Vigreux column. 4-benzyloxybutanal is obtained, b.p.0.1 =72°-73°.
후처리
- customThe supernatant dichloromethane phase is decanted off
- concentrationconcentrated by evaporation in a rotary evaporator
- filtrationThe residue is filtered over 100 g of silica gel
- concentrationThe product fractions are concentrated by evaporation in a rotary evaporator
- distillationdistilled under a high vacuum over a 10 cm Vigreux column
출처 및 근거
- ORD 기록
- ord-55e2f4e69a324d91bf8b03c727c1b3b5
- 출처 데이터셋
- uspto-grants-1994_03
- 특허 번호
- US05294734
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