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Sodium Hydroxide → HCID 44548573, 화합물

HRID 1512909
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HRID 1512909 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C:12]2[O:16][N:15]=[C:14]([C:17]3[CH:18]=[CH:19][CH:20]=[C:21]4[C:25]=3[NH:24][CH:23]=[C:22]4[CH2:26][NH:27][C@H:28]([C:30]([O:32]C)=[O:31])[CH3:29])[N:13]=2)[CH:5]=[CH:6][C:7]=1[O:8][CH:9]([CH3:11])[CH3:10].[OH-].[Na+]>O1CCCC1.CO.O>[Cl:1][C:2]1[CH:3]=[C:4]([C:12]2[O:16][N:15]=[C:14]([C:17]3[CH:18]=[CH:19][CH:20]=[C:21]4[C:25]=3[NH:24][CH:23]=[C:22]4[CH2:26][NH:27][C@H:28]([C:30]([OH:32])=[O:31])[CH3:29])[N:13]=2)[CH:5]=[CH:6][C:7]=1[O:8][CH:9]([CH3:10])[CH3:11]
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참가 물질

6

반응물 2

HCID 14798Sodium HydroxideHCID 59146180HCID 59146180, 화합물

생성물 1

HCID 44548573HCID 44548573, 화합물수율 37.9%

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 8028Tetrahydrofuran용매

반응 조건

온도
20 °C

실험 절차

To a solution of methyl N-{[7-(5-{3-chloro-4-[(1-methylethyl)oxy]phenyl}-1,2,4-oxadiazol-3-yl)-1H-indol-3-yl]methyl}-L-alaninate (D76) (223 mg) in tetrahydrofuran (5 mL) and methanol (5 mL) stirred at 20° C. was added a solution of sodium hydroxide (60 mg) in water (5 mL) in one charge. The reaction mixture was stirred at 20° C. overnight. The reaction mixture was concentrated to about 5 mL and then HCl aquous solution was added dropwise until no further white precipitate was formed. The solid was filtered and washed with EtOAc. The solid was collected and then was suspended in methanol (5 mL) and water (5 mL). The mixture was acidified with HCl (1 M) solution to pH around 1 to form a clear solution. After most of the solvent was evaporated off, the residue was freeze-dried to afford N-{[7-(5-{3-chloro-4-[(1-methylethyl)oxy]phenyl}-1,2,4-oxadiazol-3-yl)-1H-indol-3-yl]methyl}-L-alanine (E50) (82 mg) as a hydrochloride salt. δH (DMSO-d6, 400 MHz): 1.34 (3H, d), 1.38 (6H, d), 3.33 (1H, m), 4.28 (2H, q), 4.88-4.94 (1H, m), 7.31 (1H, t), 7.47 (1H, d), 7.64 (1H, d), 8.00 (1H, d), 8.05 (1H, d), 8.22 (1H, dd), 8.40 (1H, d), 11.26 (1H, br s). MS (ES): C23H23ClN4O4 requires 454; found 366.1 (M—NHC2H3COOH+).

후처리

  1. additioncharge
  2. concentrationThe reaction mixture was concentrated to about 5 mL
  3. additionHCl aquous solution was added dropwise until no further white precipitate
  4. customwas formed
  5. filtrationThe solid was filtered
  6. washwashed with EtOAc
  7. customThe solid was collected
  8. customto form a clear solution
  9. customAfter most of the solvent was evaporated off
  10. customthe residue was freeze-dried

출처 및 근거

ORD 기록
ord-6fa3c814c0f141849371d3926ec93e58
출처 데이터셋
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08217028B2

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