Sodium sulfate decahydrate → 3-(2-Methoxy-phenyl)-propan-1-ol

HRID 743384

반응식

HRID 743384 반응식
[CH3:1][O:2][C:3]1[CH:15]=[CH:14][CH:13]=[CH:12][C:4]=1[CH:5]=[CH:6][C:7](OCC)=[O:8].[H-].[Al+3].[Li+].[H-].[H-].[H-].O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+].[H-]>O1CCCC1>[CH3:1][O:2][C:3]1[CH:15]=[CH:14][CH:13]=[CH:12][C:4]=1[CH2:5][CH2:6][CH2:7][OH:8]

참가 물질

6

반응물 4

HCID 62649Sodium sulfate decahydrateHCID 90485Ethyl 3-(2-methoxyphenyl)prop-2-enoateHCID 166653HydrideHCID 21226445Aluminium lithium hydride

생성물 1

HCID 2549583-(2-Methoxy-phenyl)-propan-1-ol수율 81%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of 980 mg of ethyl 2-methoxycinnamate in 15 ml of tetrahydrofuran was added dropwise to a dispersion of 290 mg of lithium aluminum hydride and 10 ml of tetrahydrofuran, whilst ice-cooling. After the addition was complete, the reaction mixture was stirred at room temperature for 1.5 hours, and then sufficient sodium sulfate decahydrate was slowly added, whilst ice-cooling, to the mixture in order to decompose any excess of the hydride. Insoluble materials were filtered off, and the filtrate was concentrated by distillation under reduced pressure. The resulting residue was purified by column chromatography through silica gel, using a 3:1 by volume mixture of hexane and ethyl acetate as the eluent, to give 640 mg of 3-(2-methoxyphenyl)propanol as a colorless oil.

후처리

  1. temperaturecooling
  2. additionAfter the addition
  3. temperaturecooling, to the mixture in order
  4. filtrationInsoluble materials were filtered off
  5. concentrationthe filtrate was concentrated by distillation under reduced pressure
  6. customThe resulting residue was purified by column chromatography through silica gel
  7. additionby volume mixture of hexane and ethyl acetate as the eluent

출처 및 근거

ORD 기록
ord-88cc5d468bbc4a44826ea7d8588e3aeb
출처 데이터셋
uspto-grants-1996_09
특허 번호
US05556864

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