Dimethylformamide → HCID 20399003, 화합물

HRID 1981281노트

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HRID 1981281 반응식
CN(C)C=O.[C:6]([C:8]1[C:13]([C:14]#[N:15])=[C:12]([CH2:16][CH2:17][CH2:18][CH2:19][CH3:20])[CH:11]=[CH:10][C:9]=1[OH:21])#[N:7].C(=O)([O-])[O-].[K+].[K+].[CH2:28]([C:31]12[CH2:38][CH2:37][C:34]([CH2:39]Br)([CH2:35][CH2:36]1)[CH2:33][CH2:32]2)[CH2:29][CH3:30]>O>[C:6]([C:8]1[C:13]([C:14]#[N:15])=[C:12]([CH2:16][CH2:17][CH2:18][CH2:19][CH3:20])[CH:11]=[CH:10][C:9]=1[O:21][CH2:39][C:34]12[CH2:35][CH2:36][C:31]([CH2:28][CH2:29][CH3:30])([CH2:38][CH2:37]1)[CH2:32][CH2:33]2)#[N:7]

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 203989701-(Bromomethyl)-4-propylbicyclo[2.2.2]octaneHCID 203990393-Hydroxy-6-pentylbenzene-1,2-dicarbonitrile

생성물 1

HCID 20399003HCID 20399003, 화합물

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
80 °C

실험 절차

50 ml of dimethylformamide were added to 0.04 mole of 2,3-dicyano-4-pentylphenol, 0.2 mole of potassium carbonate and 0.04 mole of 4-propyl-1-bicyclo(2,2,2)-octylmethyl bromide. The mixture was stirred at 80° C. for 48 hours. The mixture was then cooled to room temperature and poured into 200 ml of water and the organic phase was extracted. The organic extract was washed with water and dried over magnesium sulfate. After the solvent had been evaporated off, the crude product was recrystallized several times. The pure product has a high melting point of 133.1° C. and a negative DCA.

후처리

  1. temperatureThe mixture was then cooled to room temperature
  2. extractionthe organic phase was extracted
  3. extractionThe organic extract
  4. washwas washed with water
  5. dry with materialdried over magnesium sulfate
  6. customAfter the solvent had been evaporated off
  7. customthe crude product was recrystallized several times

출처 및 근거

ORD 기록
ord-6543fd1f774448baae67055298b1c141
출처 데이터셋
uspto-grants-1985_04
특허 번호
US04514317

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