Potassium Carbonate → HCID 57145772, 화합물

HRID 1285134

반응식

HRID 1285134 반응식
[NH2:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[C:4](Cl)[N:3]=1.[F:12][C:13]1[CH:18]=[CH:17][C:16]([C:19]2([CH2:24][CH2:25][CH2:26][N:27]3[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]3)[O:23][CH2:22][CH2:21][O:20]2)=[CH:15][CH:14]=1.C(=O)([O-])[O-].[K+].[K+]>C(O)CC>[CH2:21]1[O:20][C:19]([C:16]2[CH:17]=[CH:18][C:13]([F:12])=[CH:14][CH:15]=2)([CH2:24][CH2:25][CH2:26][N:27]2[CH2:28][CH2:29][N:30]([C:4]3[N:3]=[C:2]([NH2:1])[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=3)[CH2:31][CH2:32]2)[O:23][CH2:22]1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 27240356-Chloro-3-nitropyridin-2-ylamineHCID 27831211-(3-(2-(4-Fluorophenyl)-1,3-dioxolan-2-yl)propyl)piperazine

생성물 1

HCID 57145772HCID 57145772, 화합물

시약·촉매·용매 1

HCID 10311-Propanol용매

실험 절차

5.6 g 2-amino-6-chloro-3-nitropyridine, 10 g 1-(3-[2-(4-fluorophenyl)-1,3-dioxolan-2-yl]-propyl)piperazine, 5 g potassium carbonate and 100 ml n-propanol are refluxed 21/2 hours. After cooling the precipitate is filtered off. The filtrate is concentrated to ca. 10 ml and diluted with the same volume of diisopropyl ether. The resulting cristallisate is admixed with the above mentioned precipitate and partitioned between water and methylene chloride. The organic phase is filtered and evaporated to give the heading compound, m.p. 117°-118°.

후처리

  1. temperatureAfter cooling the precipitate
  2. filtrationis filtered off
  3. concentrationThe filtrate is concentrated to ca. 10 ml
  4. additiondiluted with the same volume of diisopropyl ether
  5. custompartitioned between water and methylene chloride
  6. filtrationThe organic phase is filtered
  7. customevaporated
  8. customto give the heading compound, m.p. 117°-118°

출처 및 근거

ORD 기록
ord-c37eaf3eae08407a8b0553640c833c89
출처 데이터셋
uspto-grants-1986_01
특허 번호
US04565816

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