Methanol → HCID 67453617, 화합물

HRID 1474085노트

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HRID 1474085 반응식
[Na].F[C:3]1[N:8]=[C:7]([C:9]2([C:13]#[N:14])[CH2:12][CH2:11][CH2:10]2)[CH:6]=[CH:5][CH:4]=1.[CH3:15][OH:16]>>[CH3:15][O:16][C:3]1[N:8]=[C:7]([C:9]2([C:13]#[N:14])[CH2:12][CH2:11][CH2:10]2)[CH:6]=[CH:5][CH:4]=1

참가 물질

4

반응물 3

HCID 887MethanolHCID 5360545SodiumHCID 67452252HCID 67452252, 화합물

생성물 1

HCID 67453617HCID 67453617, 화합물수율 97%

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온도
75 °C

실험 절차

To anhydrous methanol (6.0 mL) at 0° C. under nitrogen was added sodium metal (˜1 g) and the mixture stirred for 30 minutes. To the reaction mixture was added 1-(6-fluoropyridin-2-yl)cyclobutanecarbonitrile (1.6 g, 9.1 mmol) followed by heating to 75° C. and stirring for 45 minutes. The solution was cooled to room temperature and partitioned between water and EtOAc. The layers were separated, the aqueous phase was extracted with EtOAc, and the combined organic phases were washed with saturated NaCl, dried over Na2SO4, and concentrated in vacuo to give the desired product (1.7 g, 97%) as a colorless oil.

후처리

  1. stirringstirring for 45 minutes
  2. temperatureThe solution was cooled to room temperature
  3. custompartitioned between water and EtOAc
  4. customThe layers were separated
  5. extractionthe aqueous phase was extracted with EtOAc
  6. washthe combined organic phases were washed with saturated NaCl
  7. dry with materialdried over Na2SO4
  8. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-57a2c1aae25a411ebf83bb8807253340
출처 데이터셋
uspto-grants-2015_04
특허 번호
US09018223B2

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