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1,2-Dibromoethane → 5-Methyl-3,4-dihydro-2H-benzo[1,4]oxazine

HRID 1515342
ノート
印刷プレビュー

反応式

HRID 1515342 の反応式
[NH2:1][C:2]1[C:7]([OH:8])=[CH:6][CH:5]=[CH:4][C:3]=1[CH3:9].C(=O)([O-])[O-].[K+].[K+].Br[CH2:17][CH2:18]Br>CN(C)C=O>[CH3:9][C:3]1[C:2]2[NH:1][CH2:17][CH2:18][O:8][C:7]=2[CH:6]=[CH:5][CH:4]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 78391,2-Dibromoethane3 回HCID 11430Potassium CarbonateHCID 30141382-Amino-m-cresol

生成物 1

HCID 208717955-Methyl-3,4-dihydro-2H-benzo[1,4]oxazine

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
130 °C

実験手順

To a solution of 2-amino-m-cresol (5.0 g) in N,N-dimethylformamide (50 ml), potassium carbonate (28.3 g) and 1,2-dibromoethane (5.3 ml) were added and stirred at 130° C. for 4 hours and then stirred overnight at room temperature. To the reaction mixture, 1,2-dibromoethane (5.3 ml) was added and stirred at 130° C. for 6 hours. After addition of additional 1,2-dibromoethane (3.5 ml), the reaction mixture was stirred at 130° C. for 5 hours and then stirred overnight at room temperature. After insoluble materials were filtered off, the filtrate was diluted with ethyl acetate and washed sequentially with water and brine. The organic layer was dried over anhydrous sodium sulfate and then filtered to remove the desiccant, followed by distilling off the solvent under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluting solvent: n-hexane:ethyl acetate=20:1 to 10:1) to give the titled compound, i.e., 5-methyl-3,4-dihydro-2H-1,4-benzoxazine (2.69 g) as a brown oil.

後処理

  1. stirringstirred overnight at room temperature
  2. stirringstirred at 130° C. for 6 hours
  3. stirringthe reaction mixture was stirred at 130° C. for 5 hours
  4. stirringstirred overnight at room temperature
  5. filtrationAfter insoluble materials were filtered off
  6. additionthe filtrate was diluted with ethyl acetate
  7. washwashed sequentially with water and brine
  8. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  9. filtrationfiltered
  10. customto remove the desiccant
  11. distillationby distilling off the solvent under reduced pressure
  12. customThe resulting residue was purified by silica gel column chromatography (eluting solvent: n-hexane:ethyl acetate=20:1 to 10:1)

出典と根拠

ORDレコード
ord-55534882ddbb4533889b103442d9e50d
出典データセット
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08222417B2

反応ノート

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