Benzene → 4-[4-[[4-[(6-Chloronaphthalen-2-yl)sulfonyl]piperazin-1-yl]carbonyl]phenyl]-1-methylpyridinium iodide

HRID 352901ノート

反応式

HRID 352901 の反応式
[CH:1]1C=CC=CC=1.[Cl:7][C:8]1[CH:9]=[C:10]2[C:15](=[CH:16][CH:17]=1)[CH:14]=[C:13]([S:18]([N:21]1[CH2:26][CH2:25][N:24]([C:27](=[O:40])[C:28]3[CH:33]=[CH:32][C:31]([C:34]4[CH:39]=[CH:38][N:37]=[CH:36][CH:35]=4)=[CH:30][CH:29]=3)[CH2:23][CH2:22]1)(=[O:20])=[O:19])[CH:12]=[CH:11]2.C[I:42]>CO>[I-:42].[Cl:7][C:8]1[CH:9]=[C:10]2[C:15](=[CH:16][CH:17]=1)[CH:14]=[C:13]([S:18]([N:21]1[CH2:26][CH2:25][N:24]([C:27]([C:28]3[CH:29]=[CH:30][C:31]([C:34]4[CH:39]=[CH:38][N+:37]([CH3:1])=[CH:36][CH:35]=4)=[CH:32][CH:33]=3)=[O:40])[CH2:23][CH2:22]1)(=[O:20])=[O:19])[CH:12]=[CH:11]2

参加物

5

反応物 3

HCID 241BenzeneHCID 6328Methyl iodide2 回HCID 99572891-[(6-Chloronaphthalen-2-yl)sulfonyl]-4-[4-(pyridin-4-yl)benzoyl]piperazine

生成物 1

HCID 227108464-[4-[[4-[(6-Chloronaphthalen-2-yl)sulfonyl]piperazin-1-yl]carbonyl]phenyl]-1-methylpyridinium iodide収率 58%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

In a mixed solvent of benzene (10 ml) and methanol (10 ml), 1-[(6-chloronaphthalen-2-yl)sulfonyl]-4-[4-(pyridin-4-yl)benzoyl]piperazine (300 mg) obtained in Example A-1 was dissolved at room temperature, followed by the addition of methyl iodide (1 ml). To the resulting mixture, the same amount of methyl iodide was added three times at intervals of 24 hours, followed by heating under reflux for 4 days. The reaction mixture was distilled under reduced pressure and the residue was washed with methanol, collected by filtration and dried, whereby the title compound (229 mg, 58%) was obtained as a yellow solid.

後処理

  1. dissolutionwas dissolved at room temperature
  2. temperatureby heating
  3. temperatureunder reflux for 4 days
  4. distillationThe reaction mixture was distilled under reduced pressure
  5. washthe residue was washed with methanol
  6. filtrationcollected by filtration
  7. customdried

出典と根拠

ORDレコード
ord-4a5bc9df6c1543eba5c8cb12c49251a5
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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