Diethyl Ether → HCID 19737925, 화합물

HRID 2255835노트

반응식

HRID 2255835 반응식
[Mn]([O-])(=O)(=O)=O.C([N+](CCCC)(CCCC)CCCC)CCC.[CH:23]([C:25]1[C:33]2[C:32]3[CH:34]=[CH:35][CH:36]=[CH:37][C:31]=3[O:30][C:29]=2[CH:28]=[C:27]([Sn:38]([CH3:41])([CH3:40])[CH3:39])[CH:26]=1)=[O:24].S([O-])([O-])(=O)=[O:43].[Na+].[Na+].CCOCC>N1C=CC=CC=1>[C:23]([C:25]1[C:33]2[C:32]3[CH:34]=[CH:35][CH:36]=[CH:37][C:31]=3[O:30][C:29]=2[CH:28]=[C:27]([Sn:38]([CH3:41])([CH3:40])[CH3:39])[CH:26]=1)([OH:43])=[O:24]

참가 물질

6

반응물 4

HCID 3283Diethyl EtherHCID 24436Sodium SulfateHCID 11760202Tetrabutylammonium permanganateHCID 19737920HCID 19737920, 화합물

생성물 1

HCID 19737925HCID 19737925, 화합물수율 92%

시약·촉매·용매 1

HCID 1049Pyridine용매2회

실험 절차

A solution of tetra-n-butylammonium permanganate (5.1 g, 14.0 mmol) in anhydrous pyridine (35 mL) was transferred via cannula needle into a solution of the stannane 36 (5.0 g, 14.0 mmol) in anhydrous pyridine (35 mL) at 0° C. under a nitrogen atmosphere. The reaction was stirred for 30 min., then saturated aqueous sodium sulfate (50 mL) was added to quench the reaction. The mixture was then poured into ether and the layers separated. The organic layer was washed with 2N aqueous HCl (6 times with 100 mL), water (2 times) and then brine (2 times). The solution was dried with magnesium sulfate, then filtered and concentrated under vacuum to provide 4.8 g (92% yield) of the stannane 37 as a white solid.

후처리

  1. customto quench
  2. customthe reaction
  3. customthe layers separated
  4. washThe organic layer was washed with 2N aqueous HCl (6 times with 100 mL), water (2 times)
  5. dry with materialThe solution was dried with magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-d95222848a844216bb00fbd489615765
출처 데이터셋
uspto-grants-1993_08
특허 번호
US05240920

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