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Acetic Acid → (2-Methoxy-5-nitro-4-trimethylsilanylmethyl-phenyl)-carbamic acid tert-butyl ester

HRID 1051221
ノート
印刷プレビュー

反応式

HRID 1051221 の反応式
[C:1]([O:5][C:6](=[O:19])[NH:7][C:8]1[CH:13]=[C:12]([N+:14]([O-:16])=[O:15])[CH:11]=[CH:10][C:9]=1[O:17][CH3:18])([CH3:4])([CH3:3])[CH3:2].[CH3:20][Si:21]([CH2:24][Mg]Cl)([CH3:23])[CH3:22].ClC1C(=O)C(C#N)=C(C#N)C(=O)C=1Cl.C(O)(=O)C>C1COCC1>[C:1]([O:5][C:6](=[O:19])[NH:7][C:8]1[CH:13]=[C:12]([N+:14]([O-:16])=[O:15])[C:11]([CH2:20][Si:21]([CH3:24])([CH3:23])[CH3:22])=[CH:10][C:9]=1[O:17][CH3:18])([CH3:4])([CH3:3])[CH3:2]
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

6

反応物 4

HCID 176Acetic AcidHCID 67752,3-Dichloro-5,6-dicyano-1,4-benzoquinoneHCID 45790233Tert-butyl 2-methoxy-5-nitrophenylcarbamateHCID 178418680HCID 178418680、化合物

生成物 1

HCID 90102720(2-Methoxy-5-nitro-4-trimethylsilanylmethyl-phenyl)-carbamic acid tert-butyl ester収率 63.1%

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒
2 回

反応条件

温度
-70 °C

実験手順

A solution of (2-methoxy-5-nitro-phenyl)-carbamic acid tert-butyl ester (1.80 g, 6.71 mmol) in THF (50 mL) was added ((trimethylsilyl)methyl)magnesium chloride (2.47 g, 16.8 mmol) at −70° C. under nitrogen gas. The solution was then stirred at −70° C. for one hour. A solution of 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (3.05 g, 13.4 mmol) in THF (30 mL) was added, the reaction was warmed to 0° C. The reaction was allowed to stir at 0° C. for another hour. The reaction mixture is poured into an aqueous solution of acetic acid (50 mL, 5%). The aqueous phase was extracted three times with ethyl acetate and the combined organic layers were washed with brine and dried over magnesium sulfate. Filtration followed by concentration in vacuo gave brown oil. Flash chromatography (80/20 hexanes/ethyl acetate) afforded (2-methoxy-5-nitro-4-trimethylsilanylmethyl-phenyl)-carbamic acid tert-butyl ester (1.50 g, 63%) as a light oil.

後処理

  1. temperaturethe reaction was warmed to 0° C
  2. stirringto stir at 0° C. for another hour
  3. extractionThe aqueous phase was extracted three times with ethyl acetate
  4. washthe combined organic layers were washed with brine
  5. dry with materialdried over magnesium sulfate
  6. filtrationFiltration
  7. concentrationfollowed by concentration in vacuo
  8. customgave brown oil

出典と根拠

ORDレコード
ord-4eba50608b1e40a98a70d53d19779849
出典データセット
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09388166B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート