Potassium Carbonate → 2-[(3-Methyl-4-nitrophenoxy)methyl]pyrimidine

HRID 402691ノート

反応式

HRID 402691 の反応式
[N+:1]([C:4]1[C:5]([CH3:11])=[CH:6][C:7]([OH:10])=[CH:8][CH:9]=1)([O-:3])=[O:2].Cl.Cl[CH2:14][C:15]1[N:20]=[CH:19][CH:18]=[CH:17][N:16]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[CH3:11][C:5]1[CH:6]=[C:7]([CH:8]=[CH:9][C:4]=1[N+:1]([O-:3])=[O:2])[O:10][CH2:14][C:15]1[N:20]=[CH:19][CH:18]=[CH:17][N:16]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 174123-Methyl-4-nitrophenolHCID 200256062-(Chloromethyl)pyrimidine hydrochloride

生成物 1

HCID 867083912-[(3-Methyl-4-nitrophenoxy)methyl]pyrimidine

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 4-nitro-m-cresol (0.25 g, 1.6 mmol), 2-(chloromethyl)pyrimidine hydrochloride (0.40 g, 2.4 mmol) and potassium carbonate (0.50 g, 4.0 mmol) in N,N-dimethylformamide (6.0 mL) was stirred at 70° C. for 18 h. Cooled to ambient temperature, the reaction mixture was poured into ice water, extracted with ethyl acetate. The organic layer was washed with water and brine, dried over sodium sulfate, filtered and concentrated to afford 2-[(3-methyl-4-nitrophenoxy)methyl]pyrimidine as crude material (0.32 g, y. 81%) as solid.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with water and brine
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-c56424a77c214b8ea3f509cf6f206d72
出典データセット
uspto-grants-2014_06
特許番号
US08742113B2

反応ノート

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