Sodium Carbonate → 1-[4-(7-Chloro-4-quinolinylamino)benzenesulphonyl]-4-(4-fluorobenzoyl)piperazine

HRID 1788698ノート

反応式

HRID 1788698 の反応式
Cl.[Cl:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7]([NH:13][C:14]3[CH:19]=[CH:18][C:17]([S:20](Cl)(=[O:22])=[O:21])=[CH:16][CH:15]=3)=[CH:8][CH:9]=[N:10]2)=[CH:5][CH:4]=1.Cl.[F:25][C:26]1[CH:39]=[CH:38][C:29]([C:30]([N:32]2[CH2:37][CH2:36][NH:35][CH2:34][CH2:33]2)=[O:31])=[CH:28][CH:27]=1.C(=O)([O-])[O-].[Na+].[Na+]>C(Cl)(Cl)Cl.O>[Cl:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7]([NH:13][C:14]3[CH:19]=[CH:18][C:17]([S:20]([N:35]4[CH2:34][CH2:33][N:32]([C:30](=[O:31])[C:29]5[CH:28]=[CH:27][C:26]([F:25])=[CH:39][CH:38]=5)[CH2:37][CH2:36]4)(=[O:22])=[O:21])=[CH:16][CH:15]=3)=[CH:8][CH:9]=[N:10]2)=[CH:5][CH:4]=1

参加物

6

反応物 3

HCID 10340Sodium CarbonateHCID 201495884-(7-Chloro-4-quinolinylamino)benzenesulphonyl chloride hydrochlorideHCID 20149590(4-Fluorophenyl)(piperazin-1-yl)methanone hydrochloride

生成物 1

HCID 136083001-[4-(7-Chloro-4-quinolinylamino)benzenesulphonyl]-4-(4-fluorobenzoyl)piperazine収率 5%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6212Chloroform溶媒

実験手順

4-(7-Chloro-4-quinolinylamino)benzenesulphonyl chloride hydrochloride (7.8 g, 0.02 mol) was added portionwise with stirring to a cold mixture of 1-(4-fluorobenzoyl)piperazine hydrochloride (4.9 g, 0.02 mol) in chloroform (250 ml) and sodium carbonate (24.4 g) in water (250 ml). The cooling bath was removed and the mixture was allowed to warm to room temperature. After 1 hour the chloroform layer was separated and dried (MgSO4). The solvent was removed by evaporation to give a brown gum. Crystallisation from ethanol gave the pure title compound (0.53 g), m.p. 235°-237° C.

後処理

  1. customThe cooling bath was removed
  2. customAfter 1 hour the chloroform layer was separated
  3. dry with materialdried (MgSO4)
  4. customThe solvent was removed by evaporation
  5. customto give a brown gum
  6. customCrystallisation from ethanol

出典と根拠

ORDレコード
ord-53574dbaa76f4e1ea1aa1fc0780d1a5b
出典データセット
uspto-grants-1987_08
特許番号
US04684657

反応ノート

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