Butyl bromide → 4-n-Butoxy-3-methoxyphenylacetonitrile

HRID 620758

반응식

HRID 620758 반응식
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]#[N:10])=[CH:4][C:3]=1[O:11][CH3:12].[CH2:13](Br)[CH2:14][CH2:15][CH3:16].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O.C(OCC)C>[CH2:13]([O:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]#[N:10])=[CH:4][C:3]=1[O:11][CH3:12])[CH2:14][CH2:15][CH3:16]

참가 물질

6

반응물 3

HCID 8002Butyl bromideHCID 11430Potassium CarbonateHCID 782204-Hydroxy-3-methoxyphenylacetonitrile

생성물 1

HCID 212451184-n-Butoxy-3-methoxyphenylacetonitrile수율 104.7%

시약·촉매·용매 2

HCID 180Acetone용매HCID 3283Diethyl Ether용매

실험 절차

A mixture of 15 grams 4-hydroxy-3-methoxyphenylacetonitrile (91.91 mmol), 26.40 ml (33.59 grams) n-butyl bromide (245 mmol) and 21.17 grams potassium carbonate (153.2 mmol) in 150 ml acetone was heated to reflux under nitrogen for 18 hours. After cooling to room temperature, the mixture was diluted with diethyl ether and the inorganic salts were removed by filtration and were washed with diethyl ether. The filtrate and wash solutions were evaporated in vacuo to provide 21.11 grams of Compound 10c as a straw-colored viscous oil (99.9% yield) which was dried in vacuo at 50° C.

후처리

  1. temperaturewas heated
  2. temperatureto reflux under nitrogen for 18 hours
  3. customthe inorganic salts were removed by filtration
  4. washwere washed with diethyl ether
  5. washThe filtrate and wash solutions
  6. customwere evaporated in vacuo

출처 및 근거

ORD 기록
ord-1b030cb11fdb45739ddbe13af48d1e94
출처 데이터셋
uspto-grants-1989_04
특허 번호
US04822800

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