Potassium Cyanide → HCID 66989070, 화합물

HRID 2407764노트

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HRID 2407764 반응식
Br[C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[C:4]([O:11][CH2:12][CH3:13])[N:3]=1.[C-:14]#[N:15].[K+]>CN(C)C=O>[CH2:12]([O:11][C:4]1[N:3]=[C:2]([C:14]#[N:15])[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=1)[CH3:13]

참가 물질

4

반응물 2

HCID 9032Potassium CyanideHCID 8172142-bromo-6-ethoxy-3-nitropyridine

생성물 1

HCID 66989070HCID 66989070, 화합물수율 38.7%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
80 °C

실험 절차

To a solution of the compound prepared in Example 279 (0.317 g) in N,N-dimethylformamide (6 mL) was added potassium cyanide (0.100 g) at room temperature. The mixture was heated at 80° C. for 18 hours and then cooled to room temperature. The solids were filtered, and the filtrate diluted with ethyl acetate, washed with 1N hydrochloric acid and water. The organic layer was filtered, evaporated in vacuo and purified by column chromatography on silica gel (10-50% ethyl acetate in hexane) to obtain the title compound (0.096 g) having the following physical data.

후처리

  1. temperaturecooled to room temperature
  2. filtrationThe solids were filtered
  3. additionthe filtrate diluted with ethyl acetate
  4. washwashed with 1N hydrochloric acid and water
  5. filtrationThe organic layer was filtered
  6. customevaporated in vacuo
  7. custompurified by column chromatography on silica gel (10-50% ethyl acetate in hexane)

출처 및 근거

ORD 기록
ord-65af8d9478df47698328469f64d40e7e
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08809538B2

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