Sodium Cyanide → HCID 13501071、化合物

HRID 330261ノート

反応式

HRID 330261 の反応式
Br[CH2:2][C:3]1[C:12]([CH3:13])=[CH:11][C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=1.[C-:14]#[N:15].[Na+]>O>[CH3:13][C:12]1[C:3]([CH2:2][C:14]#[N:15])=[CH:4][C:5]2[C:10]([CH:11]=1)=[CH:9][CH:8]=[CH:7][CH:6]=2

参加物

4

反応物 2

HCID 8929Sodium CyanideHCID 27530932-(Bromomethyl)-3-methylnaphthalene

生成物 1

HCID 13501071HCID 13501071、化合物収率 99%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A suspension of 2-bromomethyl3-methylnaphthalene (2.87 g, 12.2 mmol) and NaCN (652 mg, 13.3 mmol) in CH3CH/H2O (9:1, 125 mL) was heated to reflux for 1 hour. Upon warming, the suspension became homogeneous. After cooling to room temperature, the volatiles were removed from the reaction mixture in vacuo and the residue was partitioned between 2O (150 mL) and CH2Cl2 (150 mL). The aqueous phase was extracted with CH2Cl2 (1×150 mL). The combined organic layers were dried (Na2SO4) and concentrated in vacuo to give the title compound as a white solid (2.18 g, 99%). This material was of sufficient purity to be used as such in the next step.

後処理

  1. temperaturewas heated
  2. temperatureto reflux for 1 hour
  3. temperatureUpon warming
  4. customthe volatiles were removed from the reaction mixture in vacuo
  5. customthe residue was partitioned between 2O (150 mL) and CH2Cl2 (150 mL)
  6. extractionThe aqueous phase was extracted with CH2Cl2 (1×150 mL)
  7. dry with materialThe combined organic layers were dried (Na2SO4)
  8. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-1a41d8d0dfd640d6b7d006b46d689e4b
出典データセット
uspto-grants-1990_01
特許番号
US04895861

反応ノート

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