Ethyl Acetate → HCID 66643951、化合物

HRID 1474323ノート

反応式

HRID 1474323 の反応式
[Br:1][C:2]1[C:3]([CH3:11])=[C:4]([CH2:9][OH:10])[CH:5]=[C:6]([CH3:8])[CH:7]=1.[Li+].[Cl-].C[CH2:15][O:16]C(C)=O>FC(F)(F)C(O)=O.CO.Cl[Pd]Cl>[Br:1][C:2]1[CH:7]=[C:6]([CH3:8])[C:5]2[C:15](=[O:16])[O:10][CH2:9][C:4]=2[C:3]=1[CH3:11]

参加物

7

反応物 3

HCID 8857Ethyl AcetateHCID 433294Lithium ChlorideHCID 10656303(3-bromo-2,5-dimethylphenyl)methanol

生成物 1

HCID 66643951HCID 66643951、化合物

試薬・触媒・溶媒 3

HCID 24290Palladium Chloride触媒HCID 887Methanol溶媒HCID 6422Trifluoroacetic acid溶媒

実験手順

To a solution of (3-bromo-2,5-dimethylphenyl)methanol (1.6 g, 7.4 mmol) in trifluoroacetic acid (20 mL) was added Tl(OOCF3)3 (4 g, 7.4 mmol) at r.t, then the reaction was stirred at r.t overnight under N2. The mixture was concentrated under pressure. The residue solids, LiCl (0.6 g, 14.9 mmol), MgO (0.6 g, 14.9 mmol) and PdCl2 (0.13 g, 0.74 mmol) in MeOH were stirred under CO at 1 Mpa over night. EtOAc was added to the mixture and filtered. The organic phase was concentrated to afford 5-bromo-4,7-dimethyl-2-benzofuran-1(3H)-one.

後処理

  1. concentrationThe mixture was concentrated under pressure
  2. filtrationfiltered
  3. concentrationThe organic phase was concentrated

出典と根拠

ORDレコード
ord-20e688a2251a46489fcd3c1460248650
出典データセット
uspto-grants-2015_04
特許番号
US09018211B2

反応ノート

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