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Acrylonitrile → HCID 15505591, 화합물

HRID 1747439
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HRID 1747439 반응식
[Cl-].[C:2]([CH2:5][N+:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[CH3:12])(O)=O.[C:13](#[N:16])[CH:14]=C.CCN(CC)CC>C1(C)C=CC=CC=1.O=[Mn]=O>[CH3:12][C:7]1[N:6]2[C:11]([CH:10]=[CH:9][CH:8]=1)=[C:14]([C:13]#[N:16])[CH:2]=[CH:5]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 7855AcrylonitrileHCID 8471TriethylamineHCID 30839496266-22-4

생성물 1

HCID 15505591HCID 15505591, 화합물

시약·촉매·용매 2

HCID 14801Manganese dioxide촉매HCID 1140Toluene용매

실험 절차

To a solution of crude 1-Carboxymethyl-2-methyl-pyridinium chloride (7 g, 0.037 mol) in toluene (50 mL) were added acrylonitrile (7.4 mL, 0.11 mol), MnO2 (6.5 g, 0.075 mol) and Et3N (2 mL) at room temperature under nitrogen atmosphere. The solution was heated to 90 C and was stirred at the same temperature for 12 hours. The solution was cooled down and was filtered to remove the excess MnO2. The filtrate was concentrated and the residue was purified by CombiFlash with 10% EtOAc in Hexane to afford the desirable product 5-Methyl-indolizine-1-carbonitrile, CAS: 5-Methyl-indolizine-1-carbonitrile (3 g, 52%) as a white solid.

후처리

  1. temperatureThe solution was heated to 90 C
  2. temperatureThe solution was cooled down
  3. filtrationwas filtered
  4. customto remove the excess MnO2
  5. concentrationThe filtrate was concentrated
  6. customthe residue was purified by CombiFlash with 10% EtOAc in Hexane

출처 및 근거

ORD 기록
ord-06dc95c1c4f845009c6b232b77c86aea
출처 데이터셋
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09150556B2

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