1-Butanol → 1-(Dibutoxymethyl)-2-nitrobenzene

HRID 552074ノート

反応式

HRID 552074 の反応式
[N+:1]([C:4]1[CH:11]=[CH:10][CH:9]=[CH:8][C:5]=1[CH:6]=[O:7])([O-:3])=[O:2].[CH2:12]([OH:16])[CH2:13][CH2:14][CH3:15].O.[C:18]1(C)[CH:23]=CC(S(O)(=O)=O)=[CH:20][CH:19]=1>C1(C)C=CC=CC=1>[CH2:23]([O:7][CH:6]([O:16][CH2:12][CH2:13][CH2:14][CH3:15])[C:5]1[CH:8]=[CH:9][CH:10]=[CH:11][C:4]=1[N+:1]([O-:3])=[O:2])[CH2:18][CH2:19][CH3:20]

参加物

5

反応物 3

HCID 2631-ButanolHCID 111012-NitrobenzaldehydeHCID 521998p-Toluenesulfonic acid monohydrate

生成物 1

HCID 150331791-(Dibutoxymethyl)-2-nitrobenzene

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A solution comprising 2-nitrobenzaldehyde (4.53 g, 30.0 mmol), 1-butanol (13.7 ml, 150 mmol) and toluene (60 ml) was added with p-toluene sulfonic acid monohydrate (57 mg, 0.300 mmol) and molecular sieves-4A (1 g), and refluxed for two days. The mixture was filtered through celite, washed with saturated sodium bicarbonate and saturated sodium chloride water, and then dried with anhydrous magnesium sulfate. The solution was concentrated to obtain Step 1 compound (8.43 g, quant) as a brown oily substance.

後処理

  1. temperaturerefluxed for two days
  2. filtrationThe mixture was filtered through celite
  3. washwashed with saturated sodium bicarbonate and saturated sodium chloride water
  4. dry with materialdried with anhydrous magnesium sulfate
  5. concentrationThe solution was concentrated
  6. customto obtain Step 1 compound (8.43 g, quant) as a brown oily substance

出典と根拠

ORDレコード
ord-b870e373095c4260958f2cae81581c84
出典データセット
uspto-grants-2011_05
特許番号
US07951799B2

反応ノート

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