Potassium Cyanide → 9-Anthraceneacetonitrile

HRID 910710

反応式

HRID 910710 の反応式
Cl[CH2:2][C:3]1[C:4]2[C:9]([CH:10]=[C:11]3[C:16]=1[CH:15]=[CH:14][CH:13]=[CH:12]3)=[CH:8][CH:7]=[CH:6][CH:5]=2.[C-:17]#[N:18].[K+]>C(#N)C>[CH:5]1[C:4]2[C:9](=[CH:10][C:11]3[C:16]([C:3]=2[CH2:2][C:17]#[N:18])=[CH:15][CH:14]=[CH:13][CH:12]=3)[CH:8]=[CH:7][CH:6]=1

参加物

4

反応物 2

HCID 9032Potassium CyanideHCID 323859-(Chloromethyl)anthracene

生成物 1

HCID 3156629-Anthraceneacetonitrile収率 98.1%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A solution of 9-chloromethyl-anthracene (10.0 g, 44.11 mmol) and potassium cyanide (28.72 g, 441.1 mmol) in acetonitrile (1.6 L) was heated to reflux for 2 hours. The mixture was cooled to room temperature, filtered and concentrated. The residue was dissolved in CH2Cl2, washed with water, dried over MgSO4 and concentrated to give anthracen-9-yl-acetonitrile as yellow crystals (9.40 g, 98% yield). 1H NMR (CDCl3) δ 8.53 (1H, s), 8.18 (2H, d), 8.07 (2H, d), 7.65 (2H, dd), 7.54 (2H, dd), 4.60 (2H, s).

後処理

  1. temperatureto reflux for 2 hours
  2. filtrationfiltered
  3. concentrationconcentrated
  4. dissolutionThe residue was dissolved in CH2Cl2
  5. washwashed with water
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-ff02c06772c54e708d29ce8c9393ac22
出典データセット
uspto-grants-2011_09
特許番号
US08022214B2

関連ノート

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