Triacetoxyperiodinane → HCID 68814779, 화합물

HRID 1436701노트

반응식

HRID 1436701 반응식
[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

참가 물질

4

반응물 2

HCID 159087TriacetoxyperiodinaneHCID 68816405HCID 68816405, 화합물

생성물 1

HCID 68814779HCID 68814779, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-12afa3cd1b4d4764908e5f49fda9d0f7
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07618978B2

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