1H-Indole-3-propanoic acid → HCID 21703095、化合物

HRID 1954225ノート

反応式

HRID 1954225 の反応式
[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]

参加物

4

反応物 3

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

生成物 1

HCID 21703095HCID 21703095、化合物

実験手順

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+).

後処理

  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%)

出典と根拠

ORDレコード
ord-666f7e7df59046dcaa87d853320d803d
出典データセット
uspto-grants-2000_09
特許番号
US06121307

反応ノート

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