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Potassium Carbonate → HCID 70234410, 화합물

HRID 1387453
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HRID 1387453 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

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온도
50 °C

실험 절차

To a stirred solution of 11-4 (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 11-5 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-d541471e84094916ac6951f7dbca3320
출처 데이터셋
uspto-grants-2001_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06268378B1

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