1H-Indole-3-propanoic acid → HCID 21703095, 화합물

HRID 1596774노트

반응식

HRID 1596774 반응식
[NH:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3](CCC(O)=O)=[CH:2]1.C(N1C=CN=C1)([N:17]1C=CN=C1)=O.[O:27]1C[CH2:30][CH2:29][CH2:28]1>>[NH:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH:3]=[C:2]1[CH2:30][CH2:29][C:28]([NH2:17])=[O:27]

참가 물질

4

반응물 3

HCID 37441H-Indole-3-propanoic acidHCID 8028TetrahydrofuranHCID 682631,1'-Carbonyldiimidazole

생성물 1

HCID 21703095HCID 21703095, 화합물

실험 절차

A solution of 3-indolepropionic acid (15 g, 79 mmol), 1,1′-carbonyldimidazole (16.7 g, 100 mmol) in anhydrous tetrahydrofuran (150 ml) was allowed to stir for 1.5 hours at room temperature. Then NH3 was bubbled through the solution for 2.5 hours at room temperature. The solvent was removed under vacuum, and the residue was dissolved in ethyl acetate (500 ml). The organic solution was washed with water (3×150 ml ), dried over anhydrous sodium sulfate, filtered, and the solvent was removed under vacuum. The white solid was collected and dried under vacuum 10.42 g (96%); mp 124-125° C. MS EI m/e 188 (M+)

후처리

  1. customThen NH3 was bubbled through the solution for 2.5 hours at room temperature
  2. customThe solvent was removed under vacuum
  3. dissolutionthe residue was dissolved in ethyl acetate (500 ml)
  4. washThe organic solution was washed with water (3×150 ml )
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. customthe solvent was removed under vacuum
  8. customThe white solid was collected
  9. customdried under vacuum 10.42 g (96%)

출처 및 근거

ORD 기록
ord-e745eb99dd824bbaa05cbbc58d009743
출처 데이터셋
uspto-grants-2001_09
특허 번호
US06291683B1

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