Triacetoxyperiodinane → 3-Methyl-2-nitrobenzaldehyde

HRID 1174352ノート

反応式

HRID 1174352 の反応式
[CH3:1][C:2]1[C:3]([N+:10]([O-:12])=[O:11])=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH2:5][OH:6].CC(OI1(OC(C)=O)(OC(C)=O)OC(=O)C2C=CC=CC1=2)=O>C(#N)C>[CH3:1][C:2]1[C:3]([N+:10]([O-:12])=[O:11])=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH:5]=[O:6]

参加物

4

反応物 2

HCID 159087TriacetoxyperiodinaneHCID 5619893-Methyl-2-nitrobenzenemethanol

生成物 1

HCID 135735673-Methyl-2-nitrobenzaldehyde収率 98%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A solution of 3-methyl-2-nitrobenzyl alcohol (0.4 g, 2.4 mmol) in acetonitrile (8 mL) was treated with Dess-Martin reagent (1.11 g, 2.63 mmol) at 25° C. for 16 h. The mixture was quenched with sodium bicarbonate/sodium thiosulfate (1:1, 15 mL), and the mixture was extracted with dichloromethane, the organic layer separated, washed with brine, dried over sodium sulfate, filtered, and the solvents were evaporated to give the crude title compound (0.387 g, 98%).

後処理

  1. customThe mixture was quenched with sodium bicarbonate/sodium thiosulfate (1:1, 15 mL)
  2. extractionthe mixture was extracted with dichloromethane
  3. customthe organic layer separated
  4. washwashed with brine
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. customthe solvents were evaporated

出典と根拠

ORDレコード
ord-67b24b1500684ef7803136e998954f78
出典データセット
uspto-grants-2010_11
特許番号
US07834043B2

反応ノート

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