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Dimethylformamide → HCID 89619455, 화합물

HRID 591217
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HRID 591217 반응식
[Cl:1][C:2]1[CH:3]=[C:4](C(C(O)=O)C(O)=O)[CH:5]=[C:6]([Cl:8])[CH:7]=1.Cl[CH2:17][Cl:18].[C:19](Cl)(=O)[C:20]([Cl:22])=[O:21].CN(C)C=[O:28]>>[Cl:1][C:2]1[CH:3]=[C:4]([CH:19]([C:17]([Cl:18])=[O:28])[C:20]([Cl:22])=[O:21])[CH:5]=[C:6]([Cl:8])[CH:7]=1
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참가 물질

5

반응물 4

HCID 6228DimethylformamideHCID 6344DichloromethaneHCID 65578Oxalyl chlorideHCID 73554943HCID 73554943, 화합물

생성물 1

HCID 89619455HCID 89619455, 화합물

실험 절차

A 4-necked 500-mL flask equipped with overhead stirrer, condenser, thermometer, and addition funnel was charged with 2-(3,5-dichlorophenyl)propanedioic acid (21.8 g, 87.6 mmol), anhydrous dichloromethane (300 mL), and N,N-dimethylformamide (0.1 mL). To this stirred solution was added oxalyl chloride (19 mL, 217 mmol) over 10 min at room temperature. The mixture was stirred at room temperature for 1 hr, then refluxed for 2.5 h under nitrogen. The resulting yellow solution was concentrated under reduced pressure (20 mmHg) at a temperature of 25° C. to yield the crude product as an orange oil. The resulting material was used directly in the next step.

후처리

  1. customA 4-necked 500-mL flask equipped with overhead stirrer, condenser
  2. additionthermometer, and addition funnel
  3. temperaturerefluxed for 2.5 h under nitrogen
  4. concentrationThe resulting yellow solution was concentrated under reduced pressure (20 mmHg) at a temperature of 25° C.

출처 및 근거

ORD 기록
ord-fccbe3c0aaf44316a48bea01e22bc420
출처 데이터셋
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09238650B2

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