Methyl iodide → HCID 69700396、化合物

HRID 1061074ノート

反応式

HRID 1061074 の反応式
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

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 22709656HCID 22709656、化合物

生成物 1

HCID 69700396HCID 69700396、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-97a6bcdb51c645dbb160daa80f147b90
出典データセット
uspto-grants-2003_02
特許番号
US06525042B1

反応ノート

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