Methylamine → 2,3,4-Trifluoro-N-methyl-6-nitroaniline

HRID 1258706

反応式

HRID 1258706 の反応式
[CH3:1][NH2:2].[F:3][C:4]1[CH:9]=[C:8]([N+:10]([O-:12])=[O:11])[C:7](F)=[C:6]([F:14])[C:5]=1[F:15]>C1COCC1>[F:14][C:6]1[C:5]([F:15])=[C:4]([F:3])[CH:9]=[C:8]([N+:10]([O-:12])=[O:11])[C:7]=1[NH:2][CH3:1]

参加物

4

反応物 2

HCID 6329MethylamineHCID 796912,3,4,5-Tetrafluoronitrobenzene

生成物 1

HCID 866743382,3,4-Trifluoro-N-methyl-6-nitroaniline

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
-20 °C

実験手順

A solution of MeNH2 in THF (50.7 mL, 2 M, 101 mmol) was added dropwise to a solution of 1,2,3,4-tetrafluoro-5-nitrobenzene (9.88 g, 50.7 mmol) in THF (200 mL) at −20° C. The mixture was stirred at −20° C. for 1.5 h, concentrated, washed with brine and extracted with EtOAc. The organic layer was dried over Na2SO4, filtered and concentrated. Crystallization from EtOAc/PE gave the sub-title compound. Yield: 8.5 g (81%).

後処理

  1. concentrationconcentrated
  2. washwashed with brine
  3. extractionextracted with EtOAc
  4. dry with materialThe organic layer was dried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customCrystallization from EtOAc/PE

出典と根拠

ORDレコード
ord-e60785a33adb427683e16197dd93d862
出典データセット
uspto-grants-2013_06
特許番号
US08466186B2

関連ノート

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