Sodium Cyanide → HCID 69477110、化合物

HRID 2275861

反応式

HRID 2275861 の反応式
[CH2:1]([O:8][CH2:9][C:10]([CH3:12])=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C-:13]#[N:14].[Na+].[Cl-].[NH4+:17]>N.CO.ClCCl>[NH2:17][C:10]([CH3:12])([CH2:9][O:8][CH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[C:13]#[N:14]

参加物

7

反応物 3

HCID 8929Sodium CyanideHCID 25517Ammonium ChlorideHCID 36912841-(Benzyloxy)propan-2-one

生成物 1

HCID 69477110HCID 69477110、化合物

試薬・触媒・溶媒 3

HCID 222Ammonia溶媒2 回HCID 887Methanol溶媒2 回HCID 6344Dichloromethane溶媒

実験手順

5.07 g (27.79 mmol) of 1-(benzyloxy)acetone were initially charged in 55.6 ml of 2 N aqueous ammonia in methanol, 1.53 g (31.12 mmol) of sodium cyanide and 3.71 g (31.12 mmol) of ammonium chloride were added and the mixture was heated under reflux for 2 h. Another 27.4 ml of 2 N aqueous ammonia in methanol were then added, and the reaction mixture was stirred under reflux for 2 h. The reaction solution was cooled and diluted with 90 ml of dichloromethane. The solid obtained was filtered off and the filtrate was concentrated. The residue was purified using silica gel (mobile phase: cyclohexane/ethyl acetate gradient: from 4/1 to 1/1). This gave 4.94 g of the target compound (90% pure, 84% of theory).

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 2 h
  3. temperatureunder reflux for 2 h
  4. temperatureThe reaction solution was cooled
  5. customThe solid obtained
  6. filtrationwas filtered off
  7. concentrationthe filtrate was concentrated
  8. customThe residue was purified

出典と根拠

ORDレコード
ord-73372e964c0543b0b627fc9fdc4bf173
出典データセット
uspto-grants-2015_09
特許番号
US09126998B2

関連ノート

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