Sodium Cyanide → HCID 69477110, 화합물

HRID 2275861

반응식

HRID 2275861 반응식
[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]

참가 물질

7

반응물 3

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

생성물 1

HCID 69477110HCID 69477110, 화합물

시약·촉매·용매 3

HCID 222Ammonia용매2회HCID 887Methanol용매2회HCID 6344Dichloromethane용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-73372e964c0543b0b627fc9fdc4bf173
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09126998B2

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