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Acrylonitrile → HCID 15505591、化合物

HRID 1747439
ノート
印刷プレビュー

反応式

HRID 1747439 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 7855AcrylonitrileHCID 8471TriethylamineHCID 30839496266-22-4

生成物 1

HCID 15505591HCID 15505591、化合物

試薬・触媒・溶媒 2

HCID 14801Manganese dioxide触媒HCID 1140Toluene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-06dc95c1c4f845009c6b232b77c86aea
出典データセット
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09150556B2

反応ノート

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