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Potassium Carbonate → N-(2,3-Dihydroxypropyl)-2-methylprop-2-enamide

HRID 2166456
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HRID 2166456 반응식
[NH2:1][CH2:2][CH:3]([OH:6])[CH2:4][OH:5].C([O-])([O-])=O.[K+].[K+].[CH3:13][C:14]([C:16](Cl)=[O:17])=[CH2:15]>CN(C)C=O.CO>[OH:6][CH:3]([CH2:4][OH:5])[CH2:2][NH:1][C:16](=[O:17])[C:14]([CH3:15])=[CH2:13]
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참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 13528Methacryloyl chlorideHCID 735613-Amino-1,2-propanediol

생성물 1

HCID 18783193N-(2,3-Dihydroxypropyl)-2-methylprop-2-enamide

시약·촉매·용매 2

HCID 887Methanol용매HCID 6228Dimethylformamide용매2회

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온도
0 °C

실험 절차

4.56 g of 3-amino-1,2-propanediol (0.05 mol) were dissolved in 30 ml of dimethylformamide (anhydrous). This solution, and also 13.8 g of K2CO3, were transferred to a 100 ml three-necked flask fitted with dropping funnel and gas inlet and gas outlet pipe. The mixture was cooled to 0° C. in an ice bath. 6.18 ml of methacryl chloride (0.06 mol), dissolved in 30 ml of dimethylformamide, were added dropwise over 30 minutes with moderate stirring and gentle passage of nitrogen. After stirring for a further hour with ice cooling, the mixture was allowed to warm to room temperature and was stirred for a further 30 minutes. The reaction batch was filtered through a fluted filter, and the residue was discarded. The filtrate was concentrated in a rotary evaporator until a viscous oil was produced. This oil was dissolved in 30 ml of methanol and filtered a second time, and the filtrate was again concentrated in a rotary evaporator. The residual amounts of solvent were removed in a high vacuum. The yield was 8.52 g.

후처리

  1. customfitted
  2. additionwere added dropwise over 30 minutes
  3. stirringAfter stirring for a further hour with ice cooling
  4. temperatureto warm to room temperature
  5. stirringwas stirred for a further 30 minutes
  6. filtrationThe reaction batch was filtered through
  7. filtrationa fluted filter
  8. concentrationThe filtrate was concentrated in a rotary evaporator until a viscous oil
  9. customwas produced
  10. filtrationfiltered a second time
  11. concentrationthe filtrate was again concentrated in a rotary evaporator
  12. customThe residual amounts of solvent were removed in a high vacuum

출처 및 근거

ORD 기록
ord-63c1b203390f4ae098201f97553e3bcd
출처 데이터셋
uspto-grants-1990_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04945146

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