Water → HCID 11629980, 화합물

HRID 1666034노트

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HRID 1666034 반응식
[I-].[CH3:2][S+](C)C.[OH-].[K+].[F:8][C:9]([F:22])([F:21])[C:10]1([C:13]2[CH:20]=[CH:19][C:16]([CH:17]=[O:18])=[CH:15][CH:14]=2)[N:12]=[N:11]1.O>C(#N)C>[O:18]1[CH2:2][CH:17]1[C:16]1[CH:19]=[CH:20][C:13]([C:10]2([C:9]([F:8])([F:21])[F:22])[N:11]=[N:12]2)=[CH:14][CH:15]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 14797Potassium HydroxideHCID 75127Trimethylsulfonium iodideHCID 113333594-[3-(Trifluoromethyl)-3H-diaziren-3-yl]benzaldehyde

생성물 1

HCID 11629980HCID 11629980, 화합물수율 52.7%

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

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온도
60 °C

실험 절차

0.95 g of trimethylsulfonium iodide and 0.52 g of potassium hydroxide were dissolved in 4 ml of acetonitrile, and agitated for 10 minutes at 60° C. in a nitrogen gas atmosphere. 1.00 g of 4-(3-trifluoromethyl-3H-diazirine-3-yl)benzaldehyde were added together with 5.3 ml of acetonitrile, then 0.02 g of water were added. This was agitated for one hour at 60° C. in a nitrogen gas atmosphere. After extracting with ethyl ether, the resulting substance was washed twice with water and once with saturated saline solution, then dried with anhydrous magnesium sulfate, and filtered. The solvent was removed under reduced pressure, and the resulting substance was purified by silica gel chromatography (hexane:chloroform=1:2, V/V) to obtain 0.56 g of 3-(4-oxiranylphenyl)-3-trifluoromethyl-3H-diazirine (52% yield).

후처리

  1. stirringThis was agitated for one hour at 60° C. in a nitrogen gas atmosphere
  2. extractionAfter extracting with ethyl ether
  3. washthe resulting substance was washed twice with water and once with saturated saline solution
  4. dry with materialdried with anhydrous magnesium sulfate
  5. filtrationfiltered
  6. customThe solvent was removed under reduced pressure
  7. customthe resulting substance was purified by silica gel chromatography (hexane:chloroform=1:2, V/V)

출처 및 근거

ORD 기록
ord-982c4896b47741f69dd212f3f7adf5cd
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08043666B2

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