Oxalyl chloride → HCID 87955231、化合物

HRID 2271050ノート

反応式

HRID 2271050 の反応式
[C:1](Cl)(=O)[C:2]([Cl:4])=[O:3].[CH2:7]([O:9][C:10]1C=[CH:17][C:16]([S:19]([N:22]2[CH2:27][CH2:26][N:25]([CH3:28])[CH2:24][CH2:23]2)(=[O:21])=[O:20])=[CH:15][C:11]=1C(O)=O)[CH3:8]>CN(C)C=O.ClCCl>[ClH:4].[CH2:7]([O:9][C:10]1[CH:11]=[CH:15][C:16]([S:19]([N:22]2[CH2:27][CH2:26][N:25]([CH3:28])[CH2:24][CH2:23]2)(=[O:21])=[O:20])=[CH:17][C:1]=1[C:2]([Cl:4])=[O:3])[CH3:8]

参加物

5

反応物 2

HCID 65578Oxalyl chlorideHCID 121348652-Ethoxy-5-(4-methylpiperazine-1-sulfonyl)benzoic acid

生成物 1

HCID 87955231HCID 87955231、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide触媒HCID 6344Dichloromethane溶媒

実験手順

Oxalyl chloride (11.7 ml, 134 mmol) was added dropwise to an ice cold suspension of 2-ethoxy-5(4methylpiperazin-1-ylsulphonyl)benzoic acid (EP 812845) (20.0 g, 60.9 mmol) and dimethylformamide (2 drops) in dichloromethane (200 ml) over 15 minutes, and the reaction mixture stirred at room temperature for 18 hours. The mixture was concentrated under reduced pressure, the residue triturated with ether then ethyl acetate and dried at 40° C. for 16 hours, to afford the title compound, (19.6 g; 93%).

後処理

  1. concentrationThe mixture was concentrated under reduced pressure
  2. customthe residue triturated with ether
  3. dry with materialethyl acetate and dried at 40° C. for 16 hours

出典と根拠

ORDレコード
ord-2ef000c9ef674ec48c0e6b651cb9031a
出典データセット
uspto-grants-2001_12
特許番号
US06333330B1

反応ノート

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