Triacetoxyperiodinane → HCID 84717520, compound

HRID 1498972Notes

Reaction equation

HRID 1498972 reaction equation
[CH2:1]([N:3]1[C:11]2[C:6](=[CH:7][C:8]([CH2:12][OH:13])=[CH:9][CH:10]=2)[CH:5]=[N:4]1)[CH3:2].CC(OI1(OC(C)=O)(OC(C)=O)OC(=O)C2C1=CC=CC=2)=O>ClCCl>[CH2:1]([N:3]1[C:11]2[C:6](=[CH:7][C:8]([CH:12]=[O:13])=[CH:9][CH:10]=2)[CH:5]=[N:4]1)[CH3:2]

Participants

4

Reactant 2

HCID 159087TriacetoxyperiodinaneHCID 66837890HCID 66837890, compound

Product 1

HCID 84717520HCID 84717520, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

In dichloromethane (10 ml), (1-ethyl-1H-indazol-5-yl)methanol (0.3 g, 1.70 mmol) prepared in Example 4-3 was dissolved, and 1,1,1-triacetoxy-1,1-dihydro-1,2-benziodoxol-3(1H)-one (1.0 g, 2.38 mmol) was added thereto. The mixture was stirred for 2 hours. The mixture was subjected to extraction with chloroform, and the extract was dried over anhydrous magnesium sulfate and then concentrated. The concentrate was purified by silica gel column chromatography (dichloromethane:methanol=20:1) to give the title compound.

Workup

  1. extractionThe mixture was subjected to extraction with chloroform
  2. dry with materialthe extract was dried over anhydrous magnesium sulfate
  3. concentrationconcentrated
  4. customThe concentrate was purified by silica gel column chromatography (dichloromethane:methanol=20:1)

Sources & evidence

ORD record
ord-a684acfabd6b4fa2908e8d790fa454d9
Source dataset
uspto-grants-2015_12
Patent number
US09200008B2

Reaction notes

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