Ammonium thiocyanate → (4-Ethenylphenyl)methyl thiocyanate

HRID 2214315

反応式

HRID 2214315 の反応式
[S-:1][C:2]#[N:3].[NH4+].[CH:5]([C:7]1[CH:14]=[CH:13][C:10]([CH2:11]Cl)=[CH:9][CH:8]=1)=[CH2:6]>CC(C)=O>[CH:5]([C:7]1[CH:14]=[CH:13][C:10]([CH2:11][S:1][C:2]#[N:3])=[CH:9][CH:8]=1)=[CH2:6]

参加物

4

反応物 2

HCID 15666Ammonium thiocyanateHCID 74126p-Vinylbenzyl chloride

生成物 1

HCID 15217596(4-Ethenylphenyl)methyl thiocyanate収率 59.3%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

Ammonium thiocyanate (2 equiv., 43 g, 0.50 mol) was dissolved in acetone (200 ml) and 4-vinylbenzyl chloride (43 g, 0.25 mol) was added to the reaction flask. The mixture was stirred at room temperature overnight. The reaction mixture was filtered and acetone removed under reduced pressure. The resulting product was dissolved in hexane, filtered, and the solvent removed under reduced pressure. The monomer was isolated as a red-orange, slightly viscous liquid (26 g, yield 52%). 1H NMR (CDCl3) δ (ppm) 4.13 (s, 2H), 5.29 (d, 1H), 5.76 (d, 1H), 6.67 (dd, 1H), 7.31 (m, 4H).

後処理

  1. filtrationThe reaction mixture was filtered
  2. customacetone removed under reduced pressure
  3. dissolutionThe resulting product was dissolved in hexane
  4. filtrationfiltered
  5. customthe solvent removed under reduced pressure

出典と根拠

ORDレコード
ord-887688a7701a42f2aa7cc3951afdc13b
出典データセット
uspto-grants-2006_09
特許番号
US07108033B2

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