Phosphorus oxide (P4O10) → HCID 21051547、化合物

HRID 2213557ノート

反応式

HRID 2213557 の反応式
O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O.[CH2:15]([O:17][C:18]([C:20]1[C:21]([CH2:26][CH2:27][C:28]([OH:30])=O)=[CH:22][NH:23][C:24]=1[CH3:25])=[O:19])[CH3:16]>>[CH2:15]([O:17][C:18]([C:20]1[C:21]2[CH2:26][CH2:27][C:28](=[O:30])[C:22]=2[NH:23][C:24]=1[CH3:25])=[O:19])[CH3:16]

参加物

3

反応物 2

HCID 14812Phosphorus oxide (P4O10)HCID 217287442-Methyl-3-carbethoxy-4-(3-propionic acid)pyrrole

生成物 1

HCID 21051547HCID 21051547、化合物収率 85%

反応条件

温度
70 °C

実験手順

Polyphosphoric acid (20 g) and P2O5 (1.0 g) were mixed together and heated at 70° C. for 20 min. To the mixture was added 3-(4-ethoxycarbonyl-5-methyl-3-pyrrolyl)propanoic acid (1.0 g, 4.44 mmol) and heating was continued for 20 hours. The reaction was poured into ice-water, extracted with EtOAc. The organic layer was washed with brine and sat. NaHCO3, and dried (MgSO4). After removal of the solvent, the crude product was recrystallized from CH2CI2-hexane to give (0.78 g, 85%) of 2-methyl-6-oxo-1,4,5,6-tetrahydro-cyclopenta[b]pyrrole-3-carboxylic acid ethyl ester as a white solid.

後処理

  1. temperatureheating
  2. extractionextracted with EtOAc
  3. washThe organic layer was washed with brine and sat. NaHCO3
  4. dry with materialdried (MgSO4)
  5. customAfter removal of the solvent
  6. customthe crude product was recrystallized from CH2CI2-hexane

出典と根拠

ORDレコード
ord-d14de4fd13ce47d0a1166ac42444dd83
出典データセット
uspto-grants-2006_09
特許番号
US07105562B2

反応ノート

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