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2,5-Dimethoxyaniline → [16-(t-Butyldimethylsilanyloxy)hexadecyl]-(2,5-dimethoxyphenyl)amine

HRID 1367771
ノート
印刷プレビュー

反応式

HRID 1367771 の反応式
[CH3:1][O:2][C:3]1[CH:9]=[CH:8][C:7]([O:10][CH3:11])=[CH:6][C:4]=1[NH2:5].C([Li])CCC.Br[CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][O:34][Si:35]([C:38]([CH3:41])([CH3:40])[CH3:39])([CH3:37])[CH3:36].[Cl-].[NH4+]>O1CCCC1.O1CCOCC1>[Si:35]([O:34][CH2:33][CH2:32][CH2:31][CH2:30][CH2:29][CH2:28][CH2:27][CH2:26][CH2:25][CH2:24][CH2:23][CH2:22][CH2:21][CH2:20][CH2:19][CH2:18][NH:5][C:4]1[CH:6]=[C:7]([O:10][CH3:11])[CH:8]=[CH:9][C:3]=1[O:2][CH3:1])([C:38]([CH3:39])([CH3:40])[CH3:41])([CH3:37])[CH3:36]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 76132,5-DimethoxyanilineHCID 25517Ammonium ChlorideHCID 86627057(16-Bromohexadecyloxy)-t-butyldimethylsilaneHCID 178418339Butyllithium

生成物 1

HCID 66731777[16-(t-Butyldimethylsilanyloxy)hexadecyl]-(2,5-dimethoxyphenyl)amine収率 50%

試薬・触媒・溶媒 2

HCID 8028
Tetrahydrofuran
溶媒
2 回
HCID 312751,4-Dioxane溶媒

実験手順

2,5-Dimethoxyaniline (352.3 mg) was dissolved in 20 ml of tetrahydrofuran, and then 2.3 ml of n-butyl lithium (1.0 M solution in hexane), 3 ml of a solution of (16-bromohexadecyloxy)-t-butyldimethylsilane in tetrahydrofuran, and 0.20 ml of 1,4-dioxane were added to this solution at 0° C. The reaction mixture was refluxed for 24 hours while stirring. Saturated ammonium chloride solution was added to the reaction mixture, which was then extracted three times with dichloromethane. The organic layer was washed with saline solution and dried over magnesium sulfate, and the solvent was distilled off under reduced pressure. Purification of the residue by silica gel chromatography (heptane:ethyl acetate=7:3) gave [16-(t-butyldimethylsilanyloxy)hexadecyl]-(2,5-dimethoxyphenyl)amine as a yellow oil at a 50% yield.

後処理

  1. temperatureThe reaction mixture was refluxed for 24 hours
  2. extractionwas then extracted three times with dichloromethane
  3. washThe organic layer was washed with saline solution
  4. dry with materialdried over magnesium sulfate
  5. distillationthe solvent was distilled off under reduced pressure
  6. customPurification of the residue by silica gel chromatography (heptane:ethyl acetate=7:3)

出典と根拠

ORDレコード
ord-92666152c73f4e68b19c89e26e7c9a04
出典データセット
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07893304B2

反応ノート

読み込み中…

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