Dimethylformamide → HCID 20399003、化合物

HRID 1981281ノート

反応式

HRID 1981281 の反応式
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]

参加物

6

反応物 4

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

生成物 1

HCID 20399003HCID 20399003、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
80 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6543fd1f774448baae67055298b1c141
出典データセット
uspto-grants-1985_04
特許番号
US04514317

反応ノート

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