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4-(Bromomethyl)benzonitrile → HCID 54021566, 화합물

HRID 342155
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HRID 342155 반응식
[Si:1]([O:8][CH2:9][C:10]1[N:11]=[CH:12][N:13](C(C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[CH:14]=1)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].Br[CH2:35][C:36]1[CH:41]=[CH:40][C:39]([C:42]#[N:43])=[CH:38][CH:37]=1>C(#N)C>[Si:1]([O:8][CH2:9][C:10]1[N:11]([CH2:35][C:36]2[CH:41]=[CH:40][C:39]([C:42]#[N:43])=[CH:38][CH:37]=2)[CH:12]=[N:13][CH:14]=1)([C:4]([CH3:7])([CH3:5])[CH3:6])([CH3:2])[CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 869964-(Bromomethyl)benzonitrileHCID 618241HCID 618241, 화합물

생성물 1

HCID 54021566HCID 54021566, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A solution of 4-(tert-butyldimethylsilyloxymethyl)-1-triphenylmethylimidazole (4.66 g, 10.26 mmol) and 1-bromomethyl-4-cyanobenzene (2.01 g, 10.26 mmol) in acetonitrile (50 mL) was refluxed 4 h. The reaction was cooled, acetonitrile removed in vacuo, and the residue dissolved in methanol (30 mL). This solution was refluxed for 2 h, cooled and methanol evaporated. The residue was partitioned between ethyl acetate and saturated sodium bicarbonate. The crude product was chromatographed on silica with 3% methanol in chloroform. The title compound was obtained as a white solid.

후처리

  1. temperatureThe reaction was cooled
  2. customacetonitrile removed in vacuo
  3. dissolutionthe residue dissolved in methanol (30 mL)
  4. temperatureThis solution was refluxed for 2 h
  5. temperaturecooled
  6. custommethanol evaporated
  7. customThe residue was partitioned between ethyl acetate and saturated sodium bicarbonate
  8. customThe crude product was chromatographed on silica with 3% methanol in chloroform

출처 및 근거

ORD 기록
ord-57f34b8dac5f42e7b8e82774e7177843
출처 데이터셋
uspto-grants-1999_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05856326

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