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Acrylonitrile → HCID 21100522, 화합물

HRID 1352461
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HRID 1352461 반응식
Cl.[CH3:2][CH:3]1[CH2:7][CH:6]([CH3:8])[NH:5][CH:4]1[CH2:9][OH:10].[C:11](#[N:14])[CH:12]=[CH2:13]>C(=O)([O-])[O-].[K+].[K+].C(Cl)(Cl)Cl>[CH3:2][CH:3]1[CH2:7][CH:6]([CH3:8])[N:5]([CH2:13][CH2:12][C:11]#[N:14])[CH:4]1[CH2:9][OH:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 7855AcrylonitrileHCID 21100523HCID 21100523, 화합물

생성물 1

HCID 21100522HCID 21100522, 화합물

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 11430Potassium Carbonate용매

실험 절차

The entire amount of 3,5-dimethyl-2-hydroxymethylpyrrolidine hydrochloride was dissolved in aqueous potassium carbonate solution (50 mL) and chloroform (50 mL), and acrylonitrile (20 mL) was added. The mixture was heated under reflux for 2 hr. After the completion of the reaction, the organic layer was separated and dried over magnesium sulfate. The solvent was concentrated and the obtained residue was purified by silica gel column chromatography. The fraction eluted with chloroform:methanol=40:1 was concentrated to give 3-(3,5-dimethyl-2-hydroxymethylpyrrolidin-1-yl)propionitrile (2.3 g).

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후처리

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 2 hr
  3. customAfter the completion of the reaction
  4. customthe organic layer was separated
  5. dry with materialdried over magnesium sulfate
  6. concentrationThe solvent was concentrated
  7. customthe obtained residue was purified by silica gel column chromatography
  8. washThe fraction eluted with chloroform
  9. concentrationmethanol=40:1 was concentrated

출처 및 근거

ORD 기록
ord-3b9be5de76114c238602c2dc5ed91ff2
출처 데이터셋
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07220759B2

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