Oxalyl chloride → HCID 87955231, 화합물

HRID 2271050노트

반응식

HRID 2271050 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

HCID 87955231HCID 87955231, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide촉매HCID 6344Dichloromethane용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-2ef000c9ef674ec48c0e6b651cb9031a
출처 데이터셋
uspto-grants-2001_12
특허 번호
US06333330B1

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