Potassium Carbonate → HCID 67501864, 화합물

HRID 1016711

반응식

HRID 1016711 반응식
[CH2:1]([C:16]1[CH:17]=[C:18](O)[CH:19]=[CH:20][CH:21]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13]CC.[C:23](=[O:26])([O-])[O-].[K+].[K+].[N+]([C:32]1C=[C:34]([C:40]#[N:41])[C:35](=[CH:38][CH:39]=1)[C:36]#[N:37])([O-])=O.CN1CC[CH2:45][C:44]1=O>>[CH3:44][CH2:45][CH:1]([C:16]1[CH:21]=[CH:20][C:19]([O:26][C:23]2[CH:32]=[CH:39][CH:38]=[C:35]([C:36]#[N:37])[C:34]=2[C:40]#[N:41])=[CH:18][CH:17]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH3:13]

참가 물질

5

반응물 4

HCID 11430Potassium CarbonateHCID 13387N-methyl-2-pyrrolidoneHCID 68146Hydrogenated cardanolHCID 974431,2-Benzenedicarbonitrile, 4-nitro-

생성물 1

HCID 67501864HCID 67501864, 화합물수율 84%

반응 조건

온도
90 °C

실험 절차

To a 5 liter 1-necked round bottomed flask equipped with mechanical stirrer was added 502.5 grams (1.65 mole) of 3-pentadecylphenol, 200 grams (1.45 mole) of potassium carbonate, and 2,000 grams of 1-methyl-2-pyrrolidinone (anhydrous; obtained from Aldrich Chemical Co.). The mixture was heated to 90° C. for 2 hours using a heating mantle. The reaction mixture turned dark brown. Thereafter, 250.0 grams (1.45 mole) of 4-nitrophthalonitrile (obtained from Sigma-Aldrich) was added and the mixture was maintained at 90° C. for an additional 2 hours. The hot reaction mixture was then quenched by slowly pouring it into 3 liters of deionized water. The precipitated beige suspension was stirred until it had cooled to room temperature, then was filtered. The solid was then reslurried and filtered, using about 6 liter portions of deionized water, until the water used to wash the solid product was of neutral pH. The solid was then twice reslurried in 4 liters of methanol, filtered, and vacuum dried at 40° C. to give 519.8 grams (84 percent yield) of 4-(3-pentadecyl) phenoxyphthalonitrile. The purity of this material as measured by HPLC was more than 89 percent.

후처리

  1. customTo a 5 liter 1-necked round bottomed flask equipped with mechanical stirrer
  2. temperaturethe mixture was maintained at 90° C. for an additional 2 hours
  3. customThe hot reaction mixture was then quenched
  4. additionby slowly pouring it into 3 liters of deionized water
  5. temperaturehad cooled to room temperature
  6. filtrationwas filtered
  7. filtrationfiltered
  8. washto wash the solid product
  9. filtrationfiltered
  10. customvacuum dried at 40° C.

출처 및 근거

ORD 기록
ord-a1477496591b4928b43666bcd35c70df
출처 데이터셋
uspto-grants-2002_11
특허 번호
US06476219B1

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