Triacetoxyperiodinane → HCID 68814779、化合物

HRID 1436701ノート

反応式

HRID 1436701 の反応式
[CH3:1][O:2][C:3](=[O:22])[C:4]1[CH:16]=[C:15]([CH:17]([OH:21])[CH:18]([CH3:20])[CH3:19])[CH:14]=[C:6]([C:7]([N:9]([CH3:13])[CH2:10][CH2:11][CH3:12])=[O:8])[CH:5]=1.CC(OI1(OC(C)=O)(OC(C)=O)OC(=O)C2C=CC=CC1=2)=O>ClCCl>[CH3:1][O:2][C:3](=[O:22])[C:4]1[CH:16]=[C:15]([C:17](=[O:21])[CH:18]([CH3:19])[CH3:20])[CH:14]=[C:6]([C:7]([N:9]([CH3:13])[CH2:10][CH2:11][CH3:12])=[O:8])[CH:5]=1

参加物

4

反応物 2

HCID 159087TriacetoxyperiodinaneHCID 68816405HCID 68816405、化合物

生成物 1

HCID 68814779HCID 68814779、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Dissolve 5-(1-hydroxy-2-methyl-propyl)-N-methyl-N-propyl-isophthalamic acid methyl ester (70 mg, 0.23 mmol) in dichloromethane (3 mL) and add Dess-Martin periodinane (174 mg, 0.41 mmol) at room temperature. Stir the mixture overnight and quench with 10% aqueous sodium bisulfite solution. Extract the organic layer, wash with saturated aqueous sodium chloride solution, dry (magnesium sulfate), concentrate and purify (silica gel chromatography, eluting with 30:70 ethyl acetate:hexanes) to give the title compound.

後処理

  1. customquench with 10% aqueous sodium bisulfite solution
  2. extractionExtract the organic layer
  3. washwash with saturated aqueous sodium chloride solution
  4. dry with materialdry (magnesium sulfate)
  5. concentrationconcentrate
  6. custompurify
  7. wash(silica gel chromatography, eluting with 30:70 ethyl acetate:hexanes)

出典と根拠

ORDレコード
ord-12afa3cd1b4d4764908e5f49fda9d0f7
出典データセット
uspto-grants-2009_11
特許番号
US07618978B2

反応ノート

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