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Potassium Hydroxide → HCID 28556555、化合物

HRID 2244856
ノート
印刷プレビュー

反応式

HRID 2244856 の反応式
[CH:1]1([NH:7][C:8]2[CH:13]=[CH:12][C:11]([CH3:14])=[CH:10][CH:9]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[Br:15]Br.[OH-].[K+]>C(Cl)Cl>[Br:15][C:9]1[CH:10]=[C:11]([CH3:14])[CH:12]=[CH:13][C:8]=1[NH:7][CH:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1
参加物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 14797Potassium HydroxideHCID 24408BromineHCID 11424045N-cyclohexyl-4-methylaniline

生成物 1

HCID 28556555HCID 28556555、化合物収率 94%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

In a 100-mL flask, N-cyclohexyl-4-methylaniline (2.00 g, 10.6 mmol) was dissolved in methylene chloride (20 mL) and a solution of bromine (Br2) (1.69 g, 10.6 mmol) dissolved in methylene chloride (16 ml) was injected at 0° C. for 30 minutes. Then, the solution was further stirred for 2 hours, and a 1 N aqueous KOH (20 mL) solution was added. The solution added with the aqueous solution was transferred to a separatory funnel and extracted from methylene chloride (40 mL) twice. Water was removed from the combined organic layer over MgSO4, and filtered with a glass filter. The rotary evaporator was used to remove the solvent, thereby obtaining a residue. The obtained residue was separated by column chromatography to obtain colorless oil (2.67 g, 94%).

後処理

  1. additionThe solution added with the aqueous solution
  2. customwas transferred to a separatory funnel
  3. extractionextracted from methylene chloride (40 mL) twice
  4. customWater was removed from the combined organic layer over MgSO4
  5. filtrationfiltered with a glass
  6. filtrationfilter
  7. customThe rotary evaporator
  8. customto remove the solvent
  9. customobtaining a residue
  10. customThe obtained residue was separated by column chromatography

出典と根拠

ORDレコード
ord-e9649378fa104cb7b9786ea4deb8f16e
出典データセット
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07678933B2

反応ノート

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