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Dimethylformamide → Methyl 5-cyano-4-cyclopropyl-2-methylbenzoate

HRID 541266
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HRID 541266 반응식
[CH:1]1([C:4]2[C:13](I)=[CH:12][C:7]([C:8]([O:10][CH3:11])=[O:9])=[C:6]([CH3:15])[CH:5]=2)[CH2:3][CH2:2]1.[CH3:16][N:17](C=O)C>[C-]#N.[C-]#N.[Zn+2].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>[C:16]([C:13]1[C:4]([CH:1]2[CH2:3][CH2:2]2)=[CH:5][C:6]([CH3:15])=[C:7]([CH:12]=1)[C:8]([O:10][CH3:11])=[O:9])#[N:17]
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참가 물질

5

반응물 2

HCID 6228DimethylformamideHCID 68288233Methyl 4-cyclopropyl-5-iodo-2-methylbenzoate2회

생성물 1

HCID 68288751Methyl 5-cyano-4-cyclopropyl-2-methylbenzoate수율 81%

시약·촉매·용매 2

HCID 11186Zinc cyanide (Zn(CN)2)촉매HCID 178418397HCID 178418397, 화합물촉매

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온도
100 °C

실험 절차

To a solution of methyl 4-cyclopropyl-5-iodo-2-methylbenzoate (compound 142.2, 2.00 g, 6.01 mmol, 1.00 equiv, 95%) in DMF (16 mL) was added Zn(CN)2 (890 mg, 7.58 mmol, 1.27 equiv) and Pd(PPh3)4 (731 mg, 0.630 mmol, 0.11 equiv). The resulting solution was stirred at 100° C. under nitrogen overnight. After cooling to ambient temperature, the reaction was then quenched by the addition of 100 mL of FeSO4 (aq., sat.) and diluted with ethyl acetate. The resulting mixture was stirred vigorously then filtered through celite and washed with 1 M FeSO4, water, and ethyl acetate. The layers were separated and the aqueous phase was extracted with 2×100 mL of ethyl acetate. The combined organic phases were dried over anhydrous sodium sulfate and concentrated in vacuo. The residue was purified via silica gel column chromatography with ethyl acetate/petroleum ether (1/50) as eluent to yield 1.10 g (81%) of methyl 5-cyano-4-cyclopropyl-2-methylbenzoate as a light yellow oil.

후처리

  1. temperatureAfter cooling to ambient temperature
  2. customthe reaction was then quenched by the addition of 100 mL of FeSO4 (aq., sat.)
  3. additiondiluted with ethyl acetate
  4. stirringThe resulting mixture was stirred vigorously
  5. filtrationthen filtered through celite
  6. washwashed with 1 M FeSO4, water, and ethyl acetate
  7. customThe layers were separated
  8. extractionthe aqueous phase was extracted with 2×100 mL of ethyl acetate
  9. dry with materialThe combined organic phases were dried over anhydrous sodium sulfate
  10. concentrationconcentrated in vacuo
  11. customThe residue was purified via silica gel column chromatography with ethyl acetate/petroleum ether (1/50) as eluent

출처 및 근거

ORD 기록
ord-4be2e89b9dd24c85a1f44c52da01ea3d
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08871790B2

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