6-Iodochroman-4-ol → 6-Iodochroman-4-one
反応式
[I:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[O:8][CH2:7][CH2:6][CH:5]2[OH:12].C1C=C[NH+]=CC=1.[O-][Cr](Cl)(=O)=O>C(Cl)Cl>[I:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[O:8][CH2:7][CH2:6][C:5]2=[O:12]参加物
4
実験手順
To a CH2Cl2 (300 ml) suspension of 6-iodo-4-chromanol (15 g, 54.3 mmol) and 30 g of silica gel, at r.t., was added PCC (15.2 g, 70.6 mmol) as a solid. The mixture was stirred at r.t. for 3 h at which time TLC (20% EtOAc/hexanes) indicated complete reaction. The reaction mixture was filtered through a silica gel plug and the filtrate concentrated in vacuo to yield 14.9 g (95%) of 6-iodo-2,3-dihydro-4H-chromen-4-one as a white solid consistent with the literature report (Synthesis 1997, 23-25). HRMS (ESI+) calcd for C9H7IO2 m/z 273.9492; found 273.9500.
後処理
- customreaction
- filtrationThe reaction mixture was filtered through a silica gel plug
- concentrationthe filtrate concentrated in vacuo
出典と根拠
- ORDレコード
- ord-e978b79a88c44f00a6a48564523ca0c8
- 出典データセット
- uspto-grants-2009_06
- 特許番号
- US07544717B2
反応ノート
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