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Sodium Iodide → (4-Cyano-5-methyl-4-(5-cyano-2-thienyl)hexyl]-4-[2-(3-cyanophenoxy)ethyl]piperazine

HRID 1071649
ノート
印刷プレビュー

反応式

HRID 1071649 の反応式
[C:1]([C:3]([C:11]1[S:12][C:13]([C:16]#[N:17])=[CH:14][CH:15]=1)([CH:8]([CH3:10])[CH3:9])[CH2:4][CH2:5][CH2:6]O)#[N:2].C(N(CC)CC)C.S(Cl)(C)(=O)=O.[I-].[Na+].C(=O)([O-])[O-].[K+].[K+].[C:38]([C:40]1[CH:41]=[C:42]([CH:52]=[CH:53][CH:54]=1)[O:43][CH2:44][CH2:45][N:46]1[CH2:51][CH2:50][NH:49][CH2:48][CH2:47]1)#[N:39]>C(#N)C.[Cl-].[Na+].O.CN(C)C=O.CCOCC>[C:1]([C:3]([C:11]1[S:12][C:13]([C:16]#[N:17])=[CH:14][CH:15]=1)([CH:8]([CH3:10])[CH3:9])[CH2:4][CH2:5][CH2:6][N:49]1[CH2:48][CH2:47][N:46]([CH2:45][CH2:44][O:43][C:42]2[CH:52]=[CH:53][CH:54]=[C:40]([C:38]#[N:39])[CH:41]=2)[CH2:51][CH2:50]1)#[N:2]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

11

反応物 6

HCID 5238Sodium IodideHCID 8471TriethylamineHCID 11430Potassium CarbonateHCID 31297Methanesulfonyl chlorideHCID 223936354-Cyano-4-(5-cyano-2-thienyl)-5-methylhexanolHCID 223936831-(3-Cyanophenoxyethyl)piperazine

生成物 1

HCID 10161766
(4-Cyano-5-methyl-4-(5-cyano-2-thienyl)hexyl]-4-[2-(3-cyanophenoxy)ethyl]piperazine
収率 77.3%

試薬・触媒・溶媒 4

HCID 3283Diethyl Ether溶媒HCID 6228Dimethylformamide溶媒HCID 6342Acetonitrile溶媒HCID 57417360Sodium chloride; water溶媒2 回

反応条件

温度
0 °C

実験手順

In acetonitrile (10.0 ml) was dissolved 400 mg (1.61 mmol) of 4-cyano-5-methyl-4-(5-cyano-2-thienyl)hexanol, followed by cooling to 0° C. To the mixture were added 0.26 ml (1.85 mmol) of triethylamine and 0.14 ml (1.77 mmol) of mesyl chloride, followed by heating to room temperature. After 20 minutes, ether and brine were added thereto. The ether layer was washed with an aqueous saturated sodium bicarbonate and dried over anhydrous magnesium sulfate. The solvent was evaporated, to give a crude product. The half amount (ca. 0.1 mmol) of the crude mesyl compound was dissolved in 8.00 ml of dimethylformamide. To the mixture were added 724 mg (4.83 mmol) of sodium iodide, ill mg (0.81 mmol) of potassium carbonate and 243 mg (1.05 mmol) of 1-[2-(3-cyanophenoxy)ethyl]piperazine, followed by heating to 60° C. After completion of the reaction, brine was added thereto, and the objective product was extracted with ethyl acetate. The organic layer was washed with brine, and then dried over anhydrous magnesium sulfate. The solvent was evaporated, to give a crude product. The crude product was subjected to Cromatorex NH silica gel (eluted with ethyl acetate/hexane=1/1), to give 289 mg (0.63 mmol, 77.3%) of the title compound as a yellow syrup.

後処理

  1. temperatureby heating to room temperature
  2. washThe ether layer was washed with an aqueous saturated sodium bicarbonate
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was evaporated
  5. customto give a crude product
  6. temperatureby heating to 60° C
  7. additionwas added
  8. extractionthe objective product was extracted with ethyl acetate
  9. washThe organic layer was washed with brine
  10. dry with materialdried over anhydrous magnesium sulfate
  11. customThe solvent was evaporated
  12. customto give a crude product

出典と根拠

ORDレコード
ord-86f813d40c0f4e71b8735832510cefeb
出典データセット
uspto-grants-2005_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06906072B1

反応ノート

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