Methyl iodide → HCID 69700396, 화합물

HRID 1061074노트

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HRID 1061074 반응식
Cl.[Cl:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[CH:9]=[C:8]([S:13]([N:16]1[CH2:21][CH2:20][N:19]([C:22]([C:24]3[S:25][C:26]4[CH2:27][NH:28][CH:29]([CH3:33])[CH2:30][C:31]=4[N:32]=3)=[O:23])[CH2:18][CH2:17]1)(=[O:15])=[O:14])[CH:7]=[CH:6]2.C[I:35].[C:36](=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[I-:35].[Cl:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[CH:9]=[C:8]([S:13]([N:16]1[CH2:17][CH2:18][N:19]([C:22]([C:24]3[S:25][C:26]4[CH2:27][NH:28][C:29]([CH3:36])([CH3:33])[CH2:30][C:31]=4[NH+:32]=3)=[O:23])[CH2:20][CH2:21]1)(=[O:14])=[O:15])[CH:7]=[CH:6]2

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 22709656HCID 22709656, 화합물

생성물 1

HCID 69700396HCID 69700396, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
80 °C

실험 절차

In N,N-dimethylformamide (20 ml), 1-[(6-chloronaphthalen-2-yl)sulfonyl]-4-[(6-methyl-4,5,6,7-tetrahydrothiazolo[5,4-c]pyridin-2-yl)carbonyl]piperazine hydrochloride (200 mg) was dissolved, followed by the addition of methyl iodide (0.05 ml) and potassium carbonate (79 mg). The resulting mixture was stirred overnight at 80° C. After the reaction mixture was concentrated under reduced pressure, the residue was added with water and the resulting precipitate was collected by filtration. The precipitate was then dissolved in a mixed solvent (1:1) of dichloromethane and methanol, followed by the addition of ethyl acetate. The resulting precipitate was collected by filtration, whereby the title compound (144 mg, 56%) was obtained.

후처리

  1. concentrationAfter the reaction mixture was concentrated under reduced pressure
  2. additionthe residue was added with water
  3. filtrationthe resulting precipitate was collected by filtration
  4. dissolutionThe precipitate was then dissolved in a mixed solvent (1:1) of dichloromethane and methanol
  5. additionfollowed by the addition of ethyl acetate
  6. filtrationThe resulting precipitate was collected by filtration, whereby the title compound (144 mg, 56%)
  7. customwas obtained

출처 및 근거

ORD 기록
ord-97a6bcdb51c645dbb160daa80f147b90
출처 데이터셋
uspto-grants-2003_02
특허 번호
US06525042B1

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