Water → HCID 70080165, 화합물

HRID 843991노트

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HRID 843991 반응식
[CH2:1]([O:8][C:9](=[O:17])[C:10]1[CH:15]=[CH:14][CH:13]=[N:12][C:11]=1Cl)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(=O)([O-])[O-].[Cs+].[Cs+].[I:24][C:25]1[CH:26]=[C:27]([OH:31])[CH:28]=[CH:29][CH:30]=1.O>CN(C)C=O>[CH2:1]([O:8][C:9](=[O:17])[C:10]1[CH:15]=[CH:14][CH:13]=[N:12][C:11]=1[O:31][C:27]1[CH:28]=[CH:29][CH:30]=[C:25]([I:24])[CH:26]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 10796Cesium carbonateHCID 122723-IodophenolHCID 2111911benzyl 2-chloropyridine-3-carboxylate

생성물 1

HCID 70080165HCID 70080165, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution 2-Chloro-nicotinic acid benzyl ester (1.7 grams, 6.86 mmole), cesium carbonate (4.5 grams, 13.7 mmole) and 3-iodophenol (1.7 grams, 7.54 mmole) in dimethylformamide (20 ml) was stirred for 2 hours at 70-80° C. The mixture was poured into 150 ml water and extracted with diethyl ether. The combined extracts were washed with water and brine, dried over MgSO4, filtered, and concentrated to an oil which was purified via flash chromatography on silica using 30% ethyl acetate/hexane as eluent (2.32 g). MW 431.24; MS (m/e) 432 (M++1).

후처리

  1. extractionextracted with diethyl ether
  2. washThe combined extracts were washed with water and brine
  3. dry with materialdried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated to an oil which
  6. customwas purified via flash chromatography on silica using 30% ethyl acetate/hexane as eluent (2.32 g)

출처 및 근거

ORD 기록
ord-26afa9a1c1ff4ad6872d57f7cddb1ae7
출처 데이터셋
uspto-grants-2002_04
특허 번호
US06380218B1

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