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Methyl chloroformate → Methyl 2-(4-cyanonaphthalen-1-yl)acetate

HRID 132689
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HRID 132689 반응식
[CH3:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]([C:12]#[N:13])=[CH:4][CH:3]=1.[Li+].CC([N-]C(C)C)C.Cl[C:23]([O:25][CH3:26])=[O:24]>C1COCC1>[CH3:26][O:25][C:23](=[O:24])[CH2:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]([C:12]#[N:13])=[CH:4][CH:3]=1
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참가 물질

5

반응물 3

HCID 6586Methyl chloroformateHCID 1420471-Cyano-4-methylnaphthaleneHCID 2724682Lithium diisopropylamide

생성물 1

HCID 59734598Methyl 2-(4-cyanonaphthalen-1-yl)acetate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

To a solution of 4-methyl-1-cyanonaphthalene (4.35 g, 25.9 mmol) in THF (100 mL) was cooled to −78° C. and treated with commercially available LDA (2 M, 60 mL). The reaction mixture was then warmed to 0° C. and maintained at 0° C. for 30 min. The resulting red-colored solution was cooled to −78° C. and methyl chloroformate (10 mL, 130 mmol) was added. The reaction mixture was stirred while warming to rt until the displacement was complete (4 h) and then quenched with sat'd NH4Cl. The THF layer was evaporated and extracted with EtOAc (3×20 mL). The EtOAc was dried over Na2SO4 and concentrated in vacuo to afford an oil.

후처리

  1. temperaturemaintained at 0° C. for 30 min
  2. temperatureThe resulting red-colored solution was cooled to −78° C.
  3. temperaturewhile warming to rt until the displacement
  4. custom(4 h)
  5. customquenched with sat'd NH4Cl
  6. customThe THF layer was evaporated
  7. extractionextracted with EtOAc (3×20 mL)
  8. dry with materialThe EtOAc was dried over Na2SO4
  9. concentrationconcentrated in vacuo
  10. customto afford an oil

출처 및 근거

ORD 기록
ord-fcac02bdec0b40e194a5e595e8dc174e
출처 데이터셋
uspto-grants-2008_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07388027B2

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