Potassium Carbonate → HCID 15020605、化合物

HRID 1493171

反応式

HRID 1493171 の反応式
[CH:1]12[CH2:8][CH:5]([CH2:6][CH2:7]1)[CH2:4][CH2:3][C:2]2=O.[F:10][C:11]1[CH:21]=[CH:20][C:14]([C:15]([CH2:17][C:18]#[N:19])=O)=[CH:13][CH:12]=1.C(=O)([O-])[O-:23].[K+].[K+]>ClC(Cl)C(Cl)Cl>[F:10][C:11]1[CH:21]=[CH:20][C:14]([C:15]2[C:3]3[CH2:4][CH:5]4[CH2:8][CH:1]([CH2:7][CH2:6]4)[C:2]=3[NH:19][C:18](=[O:23])[CH:17]=2)=[CH:13][CH:12]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 107363Bicyclo[3.2.1]octan-2-oneHCID 2783172p-Fluorobenzoylacetonitrile

生成物 1

HCID 15020605HCID 15020605、化合物

試薬・触媒・溶媒 1

HCID 65911,1,2,2-Tetrachloroethane溶媒

反応条件

温度
100 °C

実験手順

Bicyclo[3.2.1]octan-2-one (2 g) and 4-fluorobenzoylacetonitrile (2.6 g) are dissolved in 1,1,2,2-tetrachloroethane (5 ml) and thereto is added 75% polyphosphoric acid (25 g). The mixture is stirred at 80° C. for 30 minutes, at 100° C. for 1 hour, and further at 130° C. for 30 minutes. After cooling, the reaction mixture is poured into ice-water and neutralized with potassium carbonate. The precipitated crystals are collected by filtration and washed successively with water and ethyl acetate. The resultant is recrystallized from methanol to give the desired product (2.7 g), m.p.>300° C.

後処理

  1. waitfurther at 130° C. for 30 minutes
  2. temperatureAfter cooling
  3. filtrationThe precipitated crystals are collected by filtration
  4. washwashed successively with water and ethyl acetate
  5. customThe resultant is recrystallized from methanol

出典と根拠

ORDレコード
ord-d3a5ee99b987431495d38437d6e93bc1
出典データセット
uspto-grants-1991_06
特許番号
US05021421

関連ノート

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