Potassium Carbonate → HCID 15020605, 화합물

HRID 1493171노트

반응식

HRID 1493171 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 15020605HCID 15020605, 화합물

시약·촉매·용매 1

HCID 65911,1,2,2-Tetrachloroethane용매

반응 조건

온도
100 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d3a5ee99b987431495d38437d6e93bc1
출처 데이터셋
uspto-grants-1991_06
특허 번호
US05021421

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