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Cyanocyclohexane → 1-(1,3-Thiazol-2-yl)cyclohexanecarbonitrile

HRID 410667
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HRID 410667 반응식
[CH:1]1([C:7]#[N:8])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C[Si]([N-][Si](C)(C)C)(C)C.[Na+].Cl[C:20]1[S:21][CH:22]=[CH:23][N:24]=1>C1(C)C=CC=CC=1>[S:21]1[CH:22]=[CH:23][N:24]=[C:20]1[C:1]1([C:7]#[N:8])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1
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참가 물질

5

반응물 3

HCID 69834CyanocyclohexaneHCID 764292-ChlorothiazoleHCID 2724254Sodium bis(trimethylsilyl)amide

생성물 1

HCID 672482221-(1,3-Thiazol-2-yl)cyclohexanecarbonitrile수율 42.7%

시약·촉매·용매 1

HCID 1140Toluene용매2회

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온도
0 °C

실험 절차

To a solution of cyclohexanecarbonitrile (0.913 g, 8.36 mmol) in toluene (25 ml) at 0° C. was added sodium bis(trimethylsilyl)amide (1M solution in THF, 10.0 ml, 10.0 mmol) and the resulting mixture was stirred for 1 hr at 0° C. 2-Chlorothiazole (1 g, 8.36 mmol) was then added dropwise as a solution in toluene (0.5 mL) over a period of 5 minutes and the resulting mixture was allowed to warm up from 0° C. to room temperature over 16 hrs. The reaction mixture was quenched with saturated aqueous NH4Cl (20 mL), and extracted with EtOAc (2×50 mL). The combined organic layers were washed with brine (60 mL, dried (Na2SO4), filtered and concentrated under reduced pressure. The residue was purified by column chromatography on silica (gradient elution 2% to 12% EtOAc in Hexanes) to afford 1-(1,3-thiazol-2-yl)cyclohexanecarbonitrile (686 mg, 3.57 mmol, 42.7% yield) as a pale yellow oil which solidified upon standing. MS ESI: [M+H]+ m/z 193.

후처리

  1. temperatureto warm up from 0° C. to room temperature over 16 hrs
  2. customThe reaction mixture was quenched with saturated aqueous NH4Cl (20 mL)
  3. extractionextracted with EtOAc (2×50 mL)
  4. washThe combined organic layers were washed with brine (60 mL
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. customThe residue was purified by column chromatography on silica (gradient elution 2% to 12% EtOAc in Hexanes)

출처 및 근거

ORD 기록
ord-9593079bdce3433199e542a35050e48f
출처 데이터셋
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08759366B2

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