Phosphorus oxide (P4O10) → HCID 21051547, 화합물

HRID 2213557노트

반응식

HRID 2213557 반응식
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]

참가 물질

3

반응물 2

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

생성물 1

HCID 21051547HCID 21051547, 화합물수율 85%

반응 조건

온도
70 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d14de4fd13ce47d0a1166ac42444dd83
출처 데이터셋
uspto-grants-2006_09
특허 번호
US07105562B2

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