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4-Methylmorpholine → HCID 59416036, 화합물

HRID 2061866
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HRID 2061866 반응식
[CH3:1][O:2][CH2:3][CH:4]([N:8]1[C:17]2[C:12](=[CH:13][C:14]([I:18])=[CH:15][CH:16]=2)[C:11](=[O:19])[C:10]([C:20](O)=[O:21])=[CH:9]1)[CH2:5][O:6][CH3:7].[CH3:23][N:24]1[CH2:29][CH2:28][NH:27][CH2:26][CH2:25]1.OC1C2N=NNC=2C=CC=1.CN1CCOCC1.Cl.C(N=C=NCCCN(C)C)C>ClCCl>[CH3:7][O:6][CH2:5][CH:4]([N:8]1[C:17]2[C:12](=[CH:13][C:14]([I:18])=[CH:15][CH:16]=2)[C:11](=[O:19])[C:10]([C:20]([N:27]2[CH2:28][CH2:29][N:24]([CH3:23])[CH2:25][CH2:26]2)=[O:21])=[CH:9]1)[CH2:3][O:2][CH3:1]
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참가 물질

7

반응물 5

HCID 79724-MethylmorpholineHCID 531671-MethylpiperazineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 59416009HCID 59416009, 화합물2회HCID 178418300HCID 178418300, 화합물

생성물 1

HCID 59416036HCID 59416036, 화합물수율 83.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 1-(1,3-dimethoxypropan-2-yl)-6-iodo-4-oxo-1,4-dihydroquinoline-3-carboxylic acid (Intermediate 78, 300 mg, 0.72 mmol) and 1-methylpiperazine (100 mg, 1.00 mmol) in dichloromethane (50 mL) was added hydroxybenzotriazole (HOBT) (110 mg, 0.72 mmol) and N-methylmorpholine (290 mg, 2.87 mmol). The reaction mixture was stirred for 1 h at room temperature and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (EDC HCl) (234 mg, 1.29 mmol) was added. The resulting reaction mixture was stirred at room temperature over night. The reaction mixture was quenched with 2N hydrochloric acid (30 mL) and the layers were separated. The organic layer was washed with saturated sodium bicarbonate solution (40 mL), water (60 mL) and finally with brine successively and dried over anhydrous sodium sulphate, filtered and concentrated under vacuum to afford 1-(1,3-dimethoxypropan-2-yl)-6-iodo-3-[(4-methylpiperazin-1-yl)carbonyl]quinolin-4(1H)-one 300 mg (80%) as thick oil.

후처리

  1. customThe resulting reaction mixture
  2. stirringwas stirred at room temperature over night
  3. customThe reaction mixture was quenched with 2N hydrochloric acid (30 mL)
  4. customthe layers were separated
  5. washThe organic layer was washed with saturated sodium bicarbonate solution (40 mL), water (60 mL) and finally with brine successively
  6. dry with materialdried over anhydrous sodium sulphate
  7. filtrationfiltered
  8. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-93ee20268a714f50bc1736f3b628f78e
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08283361B2

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