Triacetoxyperiodinane → HCID 90021739, 화합물

HRID 1487858노트

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HRID 1487858 반응식
[CH:1]1([C:4]2[CH:12]=[CH:11][C:7]([C:8]([OH:10])=[O:9])=[CH:6][C:5]=2[CH:13]([OH:16])[CH2:14][CH3:15])[CH2:3][CH2:2]1.CC(OI1(OC(C)=O)(OC(C)=O)OC(=O)C2C=CC=CC1=2)=O>ClCCCl>[CH:1]1([C:4]2[CH:12]=[CH:11][C:7]([C:8]([OH:10])=[O:9])=[CH:6][C:5]=2[C:13](=[O:16])[CH2:14][CH3:15])[CH2:2][CH2:3]1

참가 물질

4

반응물 2

HCID 159087TriacetoxyperiodinaneHCID 90022344HCID 90022344, 화합물2회

생성물 1

HCID 90021739HCID 90021739, 화합물수율 68.3%

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

실험 절차

Into a 500-mL round-bottom flask, was placed a mixture of 4-cyclopropyl-3-(1-hydroxypropyl)benzoic acid (compound 10.5, 3.4 g, 15.44 mmol) in 1,2-dichloroethane (300 mL) and Dess-Martin periodinane (7.2 g, 16.9 mmol). The mixture was stirred for 1.5 h at room temperature and then the solids were removed with filtration. The filtrate was concentrated under reduced pressure and the residue was purified by silica gel column chromatography with ethyl acetate:PE (1:9) to methanol/ethyl acetate (20:1) as the eluent to yield 2.3 g (68%) of the title compound as a light yellow solid.

후처리

  1. customInto a 500-mL round-bottom flask, was placed
  2. customthe solids were removed with filtration
  3. concentrationThe filtrate was concentrated under reduced pressure
  4. customthe residue was purified by silica gel column chromatography with ethyl acetate

출처 및 근거

ORD 기록
ord-62ad3a6837e24e198b05946e87729db7
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09428502B2

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