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Hydrochloric Acid → 6-[5-(5-chloro-6-isopropoxy-pyridin-3-yl)-[1,2,4]oxadiazol-3-yl]-1H-indole-3-carbaldehyde

HRID 1512805
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인쇄 미리보기

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HRID 1512805 반응식
[C:1](Cl)(C(Cl)=O)=[O:2].[Cl:7][C:8]1[CH:9]=[C:10]([C:18]2[O:22][N:21]=[C:20]([C:23]3[CH:31]=[C:30]4[C:26]([CH:27]=[CH:28][NH:29]4)=[CH:25][CH:24]=3)[N:19]=2)[CH:11]=[N:12][C:13]=1[O:14][CH:15]([CH3:17])[CH3:16].Cl.[OH-].[Na+]>C(Cl)Cl.O.CN(C=O)C>[Cl:7][C:8]1[CH:9]=[C:10]([C:18]2[O:22][N:21]=[C:20]([C:23]3[CH:31]=[C:30]4[C:26]([C:27]([CH:1]=[O:2])=[CH:28][NH:29]4)=[CH:25][CH:24]=3)[N:19]=2)[CH:11]=[N:12][C:13]=1[O:14][CH:15]([CH3:17])[CH3:16]
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참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 65578Oxalyl chlorideHCID 591460766-(5-{5-chloro-6-[(1-methylethyl)oxy]-3-pyridinyl}-1,2,4-oxadiazol-3-yl)-1H-indole

생성물 1

HCID 591461746-[5-(5-chloro-6-isopropoxy-pyridin-3-yl)-[1,2,4]oxadiazol-3-yl]-1H-indole-3-carbaldehyde

시약·촉매·용매 3

HCID 962
Water
용매
HCID 6228Dimethylformamide용매
HCID 6344Dichloromethane용매2회

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온도
0 °C

실험 절차

DMF (0.28 mL) was added dropwise to a solution of (COCl)2 (0.31 mL) in DCM (9 mL) at 0° C. The resulting mixture was stirred at 0° C. for 1 hour. Then a solution of 6-(5-{3-chloro-4-[(1-methylethyl)oxy]phenyl}-1,2,4-oxadiazol-3-yl)-1H-indole (D101) (1.06 g) in DCM (30 mL) was added. The reaction mixture was warmed to RT and stirred overnight. Then water and 2 M HCl was added. After stirred for 2 hours, the mixture was neutralized with 2 M aqueous NaOH solution until pH was between 8 and 9. The organic layer was separated and washed with brine, dried over anhydrous sodium sulfate. The dried solution was concentrated. The residue was purified by column chromatography to afford 6-(5-{5-chloro-6-[(1-methylethyl)oxy]-3-pyridinyl}-1,2,4-oxadiazol-3-yl)-1H-indole-3-carbaldehyde (D102) (620 mg) as a yellow solid. δH (DMSO-d6, 400 MHz): 1.46 (6H, d), 5.51 (1H, m), 7.99 (1H, d), 8.14 (1H, d), 8.30 (1H, s), 8.42 (1H, d), 8.46 (1H, d), 8.90 (1H, d), 8.98 (1H, br s), 10.12 (1H, d).

후처리

  1. temperatureThe reaction mixture was warmed to RT
  2. stirringstirred overnight
  3. stirringAfter stirred for 2 hours
  4. customThe organic layer was separated
  5. washwashed with brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationThe dried solution was concentrated
  8. customThe residue was purified by column chromatography

출처 및 근거

ORD 기록
ord-50811fdbfcb3487ca7d9e6f747011697
출처 데이터셋
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08217028B2

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