3,4-Bis(diethoxyphosphoryl)-2,3-dihydrothiophene → HCID 59155862、化合物

HRID 1662862ノート

反応式

HRID 1662862 の反応式
[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]

参加物

4

反応物 1

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

生成物 1

HCID 59155862HCID 59155862、化合物収率 85.4%

試薬・触媒・溶媒 2

HCID 241Benzene溶媒HCID 178418406HCID 178418406、化合物溶媒

実験手順

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%).

後処理

  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%)

出典と根拠

ORDレコード
ord-46aca065eab84388a9c1436e80c8af96
出典データセット
uspto-grants-2011_10
特許番号
US08030438B2

反応ノート

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