3,4-Bis(diethoxyphosphoryl)-2,3-dihydrothiophene → HCID 59155862, 화합물

HRID 1662862노트

반응식

HRID 1662862 반응식
[CH2:1]([O:3][P:4]([CH:9]1[C:13]([P:14]([O:19][CH2:20][CH3:21])([O:16][CH2:17][CH3:18])=[O:15])=[CH:12][S:11][CH2:10]1)([O:6][CH2:7][CH3:8])=[O:5])[CH3:2]>C1C=CC=CC=1.[O-2].[Mn+4].[O-2]>[CH2:17]([O:16][P:14]([C:13]1[C:9]([P:4]([O:3][CH2:1][CH3:2])([O:6][CH2:7][CH3:8])=[O:5])=[CH:10][S:11][CH:12]=1)([O:19][CH2:20][CH3:21])=[O:15])[CH3:18]

참가 물질

4

반응물 1

HCID 866384053,4-Bis(diethoxyphosphoryl)-2,3-dihydrothiophene

생성물 1

HCID 59155862HCID 59155862, 화합물수율 85.4%

시약·촉매·용매 2

HCID 241Benzene용매HCID 178418406HCID 178418406, 화합물용매

실험 절차

In benzene, 9.740 g (112 mmols) of commercially available manganese (IV) oxide was dissolved, to which 2.010 g (5.60 mmols) of 3,4-bis(diethoxyphosphoryl)-2,3-dihydrothiophene was added at room temperature. Thereafter, the reaction mixture was heated and stirred under reflux for 29 hours. After the reaction, the reaction mixture was cooled down to room temperature and the solid was removed by celite filtration. The filtrate was distilled off under reduced pressure to remove the solvent, and the resulting crude product was purified with a silica gel column (ethyl acetate:methanol=15:1) to obtain the specified substance in the form of a brown solid at a yield of 1.700 g (yield: 85.4%).

후처리

  1. additionwas added at room temperature
  2. temperatureThereafter, the reaction mixture was heated
  3. temperatureunder reflux for 29 hours
  4. customAfter the reaction
  5. customthe solid was removed by celite filtration
  6. distillationThe filtrate was distilled off under reduced pressure
  7. customto remove the solvent
  8. customthe resulting crude product was purified with a silica gel column (ethyl acetate:methanol=15:1)
  9. customto obtain the specified substance in the form of a brown solid at a yield of 1.700 g (yield: 85.4%)

출처 및 근거

ORD 기록
ord-46aca065eab84388a9c1436e80c8af96
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08030438B2

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