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Potassium Carbonate → HCID 70234410, 화합물

HRID 850610
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인쇄 미리보기

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HRID 850610 반응식
[CH2:1]([O:3][C:4](=[O:19])[CH:5]=[CH:6][C:7]1[CH:12]=[CH:11][C:10]([NH:13][C:14](=[O:17])[CH2:15]Cl)=[C:9]([OH:18])[CH:8]=1)[CH3:2].C([O-])([O-])=O.[K+].[K+]>CN(C=O)C>[CH2:1]([O:3][C:4](=[O:19])[CH:5]=[CH:6][C:7]1[CH:12]=[CH:11][C:10]2[NH:13][C:14](=[O:17])[CH2:15][O:18][C:9]=2[CH:8]=1)[CH3:2]
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참가 물질

4

반응물 2

HCID 11430Potassium CarbonateHCID 541602373-[4-(2-Chloroacetylamino)-3-hydroxyphenyl]acrylic acid ethyl ester

생성물 1

HCID 70234410HCID 70234410, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
50 °C

실험 절차

To a stirred solution of 10-4 (4.28 g, 15.0 mmol) in DMF (50 mL) was added K2CO3 (4.50 g, 32.6 mmol). The resulting suspension was heated to 50° C. for 12 h., after which time the reaction was concentrated. The residue was partitioned between saturated NaHCO3 and EtOAc and extracted twice with EtOAc. The combined organic layers were washed with brine, dried (Na2SO4), and concentrated. Flash chromatography (silica gel; 25:75 EtOAc/hexanes) yielded 10-5 as a beige solid.

후처리

  1. concentrationafter which time the reaction was concentrated
  2. customThe residue was partitioned between saturated NaHCO3 and EtOAc
  3. extractionextracted twice with EtOAc
  4. washThe combined organic layers were washed with brine
  5. dry with materialdried (Na2SO4)
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-fba627908d8d45bb8b1416f3896d17ad
출처 데이터셋
uspto-grants-2000_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06017926

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