Potassium Carbonate → HCID 57145772、化合物

HRID 1906419

反応式

HRID 1906419 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 57145772HCID 57145772、化合物

試薬・触媒・溶媒 1

HCID 10311-Propanol溶媒

実験手順

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°.

後処理

  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°

出典と根拠

ORDレコード
ord-f420c8f9f20247daa8f01ad337014d29
出典データセット
uspto-grants-1987_03
特許番号
US04652565

関連ノート

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