Methanol → HCID 67453617, 화합물

HRID 2276743노트

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HRID 2276743 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 stirred 6.0 mL of anhydrous methanol at 0° C. under nitrogen was added sodium metal (˜1 g) and the mixture stirred for 30 minutes. To this was added 1-(6-fluoropyridin-2-yl)cyclobutanecarbonitrile (1.6 g, 9.1 mmol, 1.0 equiv) and the resulting mixture heated to 75° C. 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. temperatureThe solution was cooled to room temperature
  2. custompartitioned between water and EtOAc
  3. customThe layers were separated
  4. extractionthe aqueous phase was extracted with EtOAc
  5. washthe combined organic phases were washed with saturated NaCl
  6. dry with materialdried over Na2SO4
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-7d2b9917e7c04abab511d9037fd72260
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09133123B2

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