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Magnesium → Nitrogen

HRID 644923
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HRID 644923 반응식
[Mg].Br[C:3]1[CH:8]=[CH:7][C:6]([CH:9]2[O:14][CH2:13][CH2:12][CH2:11][O:10]2)=[CH:5][CH:4]=1.O1CCCOC1C1C=CC([Mg]Br)=CC=1.Cl[C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=1[C:36]1[N:37]=[N:38][N:39]([CH:41]2[CH2:46][CH2:45][CH2:44][CH2:43][O:42]2)[N:40]=1.ClC1C=CC=CC=1C1N(C2CCCCO2)N=NN=1>O1CCCC1.BrCCBr.COCCOC.Cl[Ni]1(Cl)[P](C2C=CC=CC=2)(C2C=CC=CC=2)CCC[P]1(C1C=CC=CC=1)C1C=CC=CC=1.[Cl-].[Zn+2].[Cl-]>[N:37]#[N:38].[O:10]1[CH2:11][CH2:12][CH2:13][O:14][CH:9]1[C:6]1[CH:7]=[CH:8][C:3]([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=2[C:36]2[N:37]=[N:38][N:39]([CH:41]3[CH2:46][CH2:45][CH2:44][CH2:43][O:42]3)[N:40]=2)=[CH:4][CH:5]=1
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참가 물질

12

반응물 5

HCID 5462224Magnesium2회HCID 110756432-(4-Bromophenyl)-1,3-dioxane2회HCID 675464055-(2-chlorophenyl)-1-(tetrahydropyran-2-yl)-1H-tetrazoleHCID 675468845-(2-Chlorophenyl)-2-(oxan-2-yl)-2H-tetrazoleHCID 178419619HCID 178419619, 화합물2회

생성물 2

HCID 947Nitrogen
HCID 686267825-(4'-[1,3]dioxan-2-yl-biphenyl-2-yl)-2-(tetrahydro-pyran-2-yl)-2H-tetrazole

시약·촉매·용매 5

HCID 78391,2-Dibromoethane촉매HCID 3007855Zincchloride촉매HCID 178418745HCID 178418745, 화합물촉매HCID 8028Tetrahydrofuran용매3회HCID 80711,2-Dimethoxyethane용매2회

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온도
10 °C

실험 절차

A suspension of magnesium turnings (2.68 g) in anhydrous tetrahydrofuran (20 mL) is cooled to 10° C. and five drops of 1,2-dibromoethane are added. 2 mL of a solution of 2-(4-bromo-phenyl)-[1,3]dioxane (24.3 g; 100 mmol) in anhydrous tetrahydrofuran (80 mL) is added at 10° C. under vigorous stirring. After the reaction starts the remainder of the solution of 2-(4-bromo-phenyl)-[1,3]dioxane is added over 90 minutes. The resulting mixture is further stirred at about 16° C. for 2 hours and at 25° C. for 75 minutes. The concentration of 4-([1,3]dioxan-2-yl)phenylmagnesium bromide in the solution above the excess of magnesium turnings is about 0.90 M. In another flask, dichloro[1,3-bis(diphenylphosphino)propane]nickel(II) (0.054 g; 0.10 mmol) is suspended in 1,2-dimethoxyethane (7.7 mL) and cooled to about 0° C. before a 0.5 M solution of zinc chloride in tetrahydrofuran (1.0 mL; 0.50 mmol) and a solution of a mixture of 5-(2-chlorophenyl)-2-(tetrahydropyran-2-yl)-2H-tetrazole and 5-(2-chlorophenyl)-1-(tetrahydropyran-2-yl)-1H-tetrazole (2.65 g; 10.0 mmol) in 1,2-dimethoxyethane (2.7 mL) are added. To the vigorously stirred resulting suspension is added at about 0° C. 13.4 mL of the above 0.90 M 4-([1,3]dioxan-2-yl)phenylmagnesium bromide solution (12.0 mmol) over one hour. The resulting brown-yellow solution is allowed to warm up and further stirred at room temperature for 3 hours. The mixture is cooled to about 0° C. and quenched with a 7.5% solution of ammonium chloride in water (20 mL). The aqueous phase is separated and extracted with ethyl acetate (50 mL). The combined organic phases are washed with water (20 mL), a 7.5 % solution of sodium carbonate in water (20 mL) and water (20 mL). The combined organic phases are evaporated in vacuo. A solution of the resulting oil in a small amount of ethyl acetate is filtered and evaporated. The resulting oil is purified by column chromatography on silica gel eluting with a 1:2 mixture of ethyl acetate and hexane to afford the main isomer (N2-isomer) 5-(4′-[1,3]dioxan-2-yl-biphenyl-2-yl2-(tetrahydro-pyran-2-yl)-2H-tetrazole as a colorless oil and the minor isomer (N1-isomer) 5-(4′-[1,3]dioxan-2-yl-biphenyl-2-yl)-1-(tetrahydro-pyran-2-yl)-1H-tetrazole as colorless crystals.

후처리

  1. additionis added over 90 minutes
  2. additionare added
  3. stirringTo the vigorously stirred
  4. customresulting suspension
  5. additionis added at about 0° C
  6. temperatureto warm up
  7. stirringfurther stirred at room temperature for 3 hours
  8. temperatureThe mixture is cooled to about 0° C.
  9. customquenched with a 7.5% solution of ammonium chloride in water (20 mL)
  10. customThe aqueous phase is separated
  11. extractionextracted with ethyl acetate (50 mL)
  12. washThe combined organic phases are washed with water (20 mL)
  13. customThe combined organic phases are evaporated in vacuo
  14. filtrationA solution of the resulting oil in a small amount of ethyl acetate is filtered
  15. customevaporated
  16. customThe resulting oil is purified by column chromatography on silica gel eluting with a 1:2 mixture of ethyl acetate and hexane

출처 및 근거

ORD 기록
ord-109df11916f14493aea77537f68c2a26
출처 데이터셋
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07700784B2

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