Sodium Hydroxide → HCID 21914113、化合物

HRID 887930ノート

反応式

HRID 887930 の反応式
[CH:1]([CH:3]1[CH2:11][C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[N:4]1[C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])=O.[C:19]([O-])(=O)[CH3:20].[NH4+:23].[OH-].[Na+]>C(O)(=O)C>[CH3:1][C:3]1[NH:4][C:1]([CH:3]2[CH2:11][C:10]3[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=3)[N:4]2[C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])=[N:23][C:11]=1[CH2:10][CH2:19][CH3:20]

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 517165Ammonium AcetateHCID 21914148HCID 21914148、化合物

生成物 1

HCID 21914113HCID 21914113、化合物収率 255.2%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

Intermediate (12) (0.00101 mole), 2-3-hexanedione (0.004 mole), and ammonium acetate (0.025 mole) were combined in acetic acid (4 ml), and immediately placed on a steam bath for 15 minutes. After 2 hours at room temperature, the reaction was poured into ice water (100 ml), basified with 3N NaOH, and extracted with diethylether (twice). The organic phases were combined, dried, filtered, and concentrated. The residue was taken up in diethylether, concentrated and then purified by prep LC, yielding 0.440 g of 1,1-dimethylethyl 2,3-dihydro-2-(5-methyl-4-propyl-1H-imidazol-2-yl)-1H-indole-1-carboxylate (compound 99).

後処理

  1. waitAfter 2 hours at room temperature
  2. extractionextracted with diethylether (twice)
  3. customdried
  4. filtrationfiltered
  5. concentrationconcentrated
  6. concentrationconcentrated
  7. custompurified by prep LC

出典と根拠

ORDレコード
ord-9b7be88917054b0997bc2a217e90de26
出典データセット
uspto-grants-2012_08
特許番号
US08247432B2

反応ノート

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