Oxalyl chloride → HCID 87955231、化合物

HRID 2186760ノート

反応式

HRID 2186760 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、化合物収率 84%

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-(4-methylpiperazin-1-ylsulphonyl)benzoic acid (EP 812845 A1) (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).

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-87308cba657645fdbe8c21f0f9bc9a46
出典データセット
uspto-grants-2002_06
特許番号
US06407114B1

反応ノート

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