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Dimethylformamide → Benzyl 5-formyl-1H-pyrrole-2-carboxylate

HRID 2375795
ノート
印刷プレビュー

反応式

HRID 2375795 の反応式
CN([CH:4]=[O:5])C.O=P(Cl)(Cl)Cl.[CH2:11]([O:18][C:19]([C:21]1[NH:22][CH:23]=[CH:24][CH:25]=1)=[O:20])[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.[C:26]([O-])(=[O:28])C.[Na+]>C(Cl)Cl.O>[CH2:11]([O:18][C:19]([C:21]1[NH:22][C:23]([CH:4]=[O:5])=[CH:24][CH:25]=1)=[O:20])[C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1.[CH2:11]([O:18][C:19]([C:21]1[NH:22][CH:23]=[C:24]([CH:26]=[O:28])[CH:25]=1)=[O:20])[C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 6228DimethylformamideHCID 24813Phosphorus oxychlorideHCID 517045Sodium AcetateHCID 8543774HCID 8543774、化合物

生成物 2

HCID 71349636Benzyl 5-formyl-1H-pyrrole-2-carboxylateHCID 841032561H-Pyrrole-2-carboxylic acid, 4-formyl-, phenylmethyl ester

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 6344Dichloromethane溶媒2 回

実験手順

To DMF (5.93 g) was added POCl3 (12.45 g) dropwise at 0° C. The mixture was warmed to RT, diluted with DCM (40 mL) and cooled again to 0° C. A solution of 1H-pyrrole-2-carboxylic acid benzyl ester (15.00 g, prepared by adopting a procedure from J. Barry, G. Bram and A. Petit, Heterocycles 1985, 23, 875-880) in DCM (40 mL) was added dropwise at such a rate that the temperature of the reaction mixture did not rise above 0° C. The reaction was the heated to reflux for 30 min whereupon it was cooled to 10° C. A solution of sodium acetate (28g) in water (90 mL) was added carefully. After stirring for 15 min the two resulting phases were separated and the aqueous phase was washed with DCM (3×75 mL). The combined organic phases were washed with saturated Na2CO3 solution and brine, dried over MgSO4 and concentrated. The residue was purified by flash column chromatography on silica (ethyl acetate/heptanes 1:2) to provide 5-formyl-1H-pyrrole-2-carboxylic acid benzyl ester (8.0 g) and 4-formyl-1H-pyrrole-2-carboxylic acid benzyl ester (4.0 g).

後処理

  1. temperaturecooled again to 0° C
  2. customdid not rise above 0° C
  3. temperatureheated
  4. temperatureto reflux for 30 min whereupon it
  5. temperaturewas cooled to 10° C
  6. customwere separated
  7. washthe aqueous phase was washed with DCM (3×75 mL)
  8. washThe combined organic phases were washed with saturated Na2CO3 solution and brine
  9. dry with materialdried over MgSO4
  10. concentrationconcentrated
  11. customThe residue was purified by flash column chromatography on silica (ethyl acetate/heptanes 1:2)

出典と根拠

ORDレコード
ord-1f1278a2b66443fe9b0921c9123a3755
出典データセット
uspto-grants-2008_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07465806B2

反応ノート

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