Methyl iodide → HCID 69700396、化合物

HRID 352941ノート

反応式

HRID 352941 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 (79.0 mg). The resulting mixture was stirred overnight at 80° C. The reaction mixture was concentrated under reduced pressure. Water was added to the residue and the precipitate so formed was collected by filtration. The precipitate was dissolved in a 1:1 mixed solution of dichloromethane and methanol. Ethyl acetate was added to the resulting solution and the precipitate thus formed was collected by filtration, whereby the title compound (144 mg, 56%) was obtained.

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. additionWater was added to the residue
  3. customthe precipitate so formed
  4. filtrationwas collected by filtration
  5. dissolutionThe precipitate was dissolved in a 1:1 mixed solution of dichloromethane and methanol
  6. additionEthyl acetate was added to the resulting solution
  7. customthe precipitate thus formed
  8. filtrationwas collected by filtration, whereby the title compound (144 mg, 56%)
  9. customwas obtained

出典と根拠

ORDレコード
ord-694ba635c88c46d38647015073759df9
出典データセット
uspto-grants-2004_06
特許番号
US06747023B1

反応ノート

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