Sodium Carbonate → HCID 13537214、化合物

HRID 235653

反応式

HRID 235653 の反応式
[NH2:1][CH:2]1[CH2:7][CH2:6][CH2:5][N:4]([CH2:8][CH3:9])[CH2:3]1.C(=O)([O-])[O-].[Na+].[Na+].Cl.[Cl:17][C:18]1[CH:27]=[C:26]2[C:21]([C:22]([NH:28][C:29]3[CH:34]=[CH:33][C:32]([S:35](Cl)(=[O:37])=[O:36])=[CH:31][CH:30]=3)=[CH:23][N:24]=[N:25]2)=[CH:20][CH:19]=1>C(Cl)(Cl)Cl.O>[Cl:17][C:18]1[CH:27]=[C:26]2[C:21]([C:22]([NH:28][C:29]3[CH:30]=[CH:31][C:32]([S:35]([NH:1][CH:2]4[CH2:7][CH2:6][CH2:5][N:4]([CH2:8][CH3:9])[CH2:3]4)(=[O:36])=[O:37])=[CH:33][CH:34]=3)=[CH:23][N:24]=[N:25]2)=[CH:20][CH:19]=1

参加物

6

反応物 3

HCID 10340Sodium CarbonateHCID 980943-amino-N-ethylpiperidineHCID 21273956HCID 21273956、化合物

生成物 1

HCID 13537214HCID 13537214、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6212Chloroform溶媒

反応条件

温度
3 °C

実験手順

3-Amino-1-ethylpiperidine (0.4 ml) in chloroform (15 ml) was treated with anhydrous sodium carbonate (2.94 g) in water (15 ml) and cooled to 3° C. The mixture was vigorously stirred and treated with 4-(7-chloro-4-cinnolinylamino)benzenesulphonylchloride hydrochloride (1.0 g). The dark orange mixture was stirred at 3° C. for 15 minutes, then at room temperature for 45 minutes. During this period the colour lightened considerably. The chloroform layer was separated and dried over magnesium sulphate. The residue on evaporation solidified when triturated with methanol, to give the title compound (0.5 g), m.p. 213°-15° C. (with decomposition).

後処理

  1. stirringThe dark orange mixture was stirred at 3° C. for 15 minutes
  2. waitDuring this period the colour lightened considerably
  3. customThe chloroform layer was separated
  4. dry with materialdried over magnesium sulphate
  5. customThe residue on evaporation
  6. customtriturated with methanol

出典と根拠

ORDレコード
ord-f64cd5b988b14d4f8e6425d0bb08320b
出典データセット
uspto-grants-1987_02
特許番号
US04640920

関連ノート

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