Sodium Hydroxide → HCID 21914113, 화합물

HRID 551407노트

반응식

HRID 551407 반응식
[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]

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 517165Ammonium AcetateHCID 21914148HCID 21914148, 화합물

생성물 1

HCID 21914113HCID 21914113, 화합물수율 255.2%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-5e436a2611b64396ade2eea34bd3e692
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07947713B2

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