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Lithium Chloride → HCID 178501137, 화합물

HRID 446749
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HRID 446749 반응식
[Cl-].[Li+].[Mg].[H-].C([Al+]CC(C)C)C(C)C.Br[C:15]1[C:16]([Cl:21])=[N:17][CH:18]=[CH:19][CH:20]=1.[CH3:22][O:23][C:24]([C@H:26]1[CH2:31][CH2:30][C@H:29]([C:32](Cl)=[O:33])[CH2:28][CH2:27]1)=[O:25]>O1CCCC1.[Cl-].[Zn+2].[Cl-].C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[CH3:22][O:23][C:24]([C@H:26]1[CH2:31][CH2:30][C@H:29]([C:32]([C:15]2[C:16]([Cl:21])=[N:17][CH:18]=[CH:19][CH:20]=2)=[O:33])[CH2:28][CH2:27]1)=[O:25]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

10

반응물 5

HCID 433294Lithium ChlorideHCID 6933243-Bromo-2-chloropyridineHCID 5462224MagnesiumHCID 21225700DiisobutylaluminumhydrideHCID 178501148HCID 178501148, 화합물

생성물 1

HCID 178501137HCID 178501137, 화합물수율 46%

시약·촉매·용매 4

HCID 8028Tetrahydrofuran촉매
HCID 3007855Zincchloride촉매
HCID 178418397HCID 178418397, 화합물촉매
HCID 8028Tetrahydrofuran용매2회

실험 절차

To a mixture of lithium chloride (0.55 g, 13 mmol) and magnesium turnings (0.63 g, 26 mmol) in dry tetrahydrofuran (34 ml) was added 1M diisobutyl aluminum hydride solution in tetrahydrofuran (0.10 ml, 0.10 mmol) at room temperature. After stirring for 5 minutes a solution of 3-bromo-2-chloro-pyridine (2.00 g, 10.4 mmol) in dry tetrahydrofuran (1 ml) was added at 0-5° C. Stirring for 1 h was followed by addition of a solution of zinc chloride (1.42 g, 10.4 mmol), which had previously been dried by melting in vacuo followed by cooling under argon, in dry tetrahydrofuran (10 ml). After stirring for 1 h the mixture was decanted into another flask by cannulation under argon. Addition of tetrakis(triphenylphosphine)palladium(0) (0.59 g, 0.51 mmol) and trans-4-chlorocarbonyl-cyclohexanecarboxylic acid methyl ester (2.10 g, 10.3 mmol) was followed by stirring at room temperature for 18 h. The mixture was partitioned between ethyl acetate (150 ml) and 0.1M aqueous hydrogen chloride solution (100 ml). The layers were separated. The aqueous layer was extracted with two 100-ml portions of ethyl acetate. The combined organic layers were dried over anhydrous sodium sulfate and concentrated to dryness. Purification by flash-chromatography with n-heptane/tert-butyl methyl ether as eluent gave the title compound (1.3 g, 46%) as yellow solid. MS m/e: 282 ([M+H]+)

후처리

  1. additionwas added at 0-5° C
  2. customhad previously been dried
  3. temperatureby cooling under argon, in dry tetrahydrofuran (10 ml)
  4. stirringAfter stirring for 1 h the mixture
  5. customwas decanted into another flask by cannulation under argon
  6. stirringby stirring at room temperature for 18 h
  7. customThe mixture was partitioned between ethyl acetate (150 ml) and 0.1M aqueous hydrogen chloride solution (100 ml)
  8. customThe layers were separated
  9. extractionThe aqueous layer was extracted with two 100-ml portions of ethyl acetate
  10. dry with materialThe combined organic layers were dried over anhydrous sodium sulfate
  11. concentrationconcentrated to dryness
  12. customPurification by flash-chromatography with n-heptane/tert-butyl methyl ether as eluent

출처 및 근거

ORD 기록
ord-44399cd0819c4b5e856d38932478d58c
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08481528B2

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