Methanol → Methyl 2-methyl-3-(methylthio)propionate

HRID 2059064노트

반응식

HRID 2059064 반응식
[CH3:1][CH:2]([CH2:7][SH:8])[C:3]([O:5][CH3:6])=[O:4].CO.F[C:12](F)(F)COP(OCC(F)(F)F)(C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.O>ClCCl>[CH3:6][O:5][C:3](=[O:4])[CH:2]([CH3:1])[CH2:7][S:8][CH3:12]

참가 물질

6

반응물 4

HCID 887MethanolHCID 962WaterHCID 49964Triphenylbis(2,2,2-trifluoroethoxy)phosphoraneHCID 107231Methyl 2-methyl-3-mercaptopropionate

생성물 1

HCID 3018979Methyl 2-methyl-3-(methylthio)propionate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of methyl 2-methyl-3-mercaptoproponate (1.34 g, 10 mmol) and methanol (0.42 g, 10 mmole) is added to a mixture of bis(2,2,2-trifluoroethoxy)triphenylphosphorane (11 mmole) [prepared in situ from triphenylphosphine (12 mmole) and sodium 2,2,2-trifluoro ethoxide (24 mmole) in dry diethyl ether (20 ml)] in dichloromethane (20 ml). After 20 hours stirring at room temperature the mixture is poured into water and extracted with ether. The ether extract is washed with 5% aqueous sodium hydroxide and dried over magnesium sulfate. The solution is evaporated, solids removed by filtration and the oily residue purified by vacuum distillation yielding methyl-3-methylthio-2-methylpropanoate.

후처리

  1. extractionextracted with ether
  2. extractionThe ether extract
  3. washis washed with 5% aqueous sodium hydroxide
  4. dry with materialdried over magnesium sulfate
  5. customThe solution is evaporated
  6. customsolids removed by filtration
  7. distillationthe oily residue purified by vacuum distillation

출처 및 근거

ORD 기록
ord-4c9aefd2c98d45e39ec0d413fec1da52
출처 데이터셋
uspto-grants-1982_03
특허 번호
US04321383

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