Water → HCID 70080165、化合物

HRID 843991ノート

反応式

HRID 843991 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 70080165HCID 70080165、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-26afa9a1c1ff4ad6872d57f7cddb1ae7
出典データセット
uspto-grants-2002_04
特許番号
US06380218B1

反応ノート

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