Triacetoxyperiodinane → HCID 90021739、化合物

HRID 1487858ノート

反応式

HRID 1487858 の反応式
[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

参加物

4

反応物 2

HCID 159087TriacetoxyperiodinaneHCID 90022344HCID 90022344、化合物2 回

生成物 1

HCID 90021739HCID 90021739、化合物収率 68.3%

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-62ad3a6837e24e198b05946e87729db7
出典データセット
uspto-grants-2016_08
特許番号
US09428502B2

反応ノート

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