Dimethyl Sulfoxide → HCID 59478041、化合物

HRID 570821ノート

反応式

HRID 570821 の反応式
[H-].[Na+].C1(C)C=CC(S([CH:12]([N+:14]#[C-])C)(=O)=O)=CC=1.[C:17](#[N:24])[CH:18]=[CH:19][CH2:20][CH2:21][CH2:22][CH3:23].CS(C)=O.[CH2:29](OCC)[CH3:30]>O>[CH2:20]([C:19]1[C:18]([C:12]#[N:14])=[CH:17][NH:24][C:29]=1[CH3:30])[CH2:21][CH2:22][CH3:23]

参加物

7

反応物 5

HCID 679Dimethyl SulfoxideHCID 3283Diethyl Ether2 回HCID 24758Sodium hydrideHCID 287344HCID 287344、化合物HCID 110528851-(1-Isocyanoethanesulfonyl)-4-methylbenzene

生成物 1

HCID 59478041HCID 59478041、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a suspension of sodium hydride (60%, 0.096 g) in diethyl ether (3 mL) were added a solution of 1-(toluene-4-sulfonyl)ethylisocyanide (0.42 g) and 2-heptenenitrile (0.22 g) in a mixed solvent of diethyl ether (3 mL) and dimethylsulfoxide (3 mL) at room temperature, and this mixture was stirred at room temperature for 1 hour. To this reaction mixture was added water (15 mL). This mixture was extracted with ethyl acetate, and this organic layer was washed with brine, and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure. The residue was purified by column chromatography on silica gel (eluent: ethyl acetate/n-hexane) to give the title compound (0.19 g).

後処理

  1. extractionThis mixture was extracted with ethyl acetate
  2. washthis organic layer was washed with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was removed under reduced pressure
  5. customThe residue was purified by column chromatography on silica gel (eluent: ethyl acetate/n-hexane)

出典と根拠

ORDレコード
ord-82461a7798fd4b4a9a52befd31b019e3
出典データセット
uspto-grants-2015_05
特許番号
US09023882B2

反応ノート

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