Ethyl Acetate → HCID 66643951, 화합물

HRID 1474323노트

반응식

HRID 1474323 반응식
[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]

참가 물질

7

반응물 3

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

생성물 1

HCID 66643951HCID 66643951, 화합물

시약·촉매·용매 3

HCID 24290Palladium Chloride촉매HCID 887Methanol용매HCID 6422Trifluoroacetic acid용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-20e688a2251a46489fcd3c1460248650
출처 데이터셋
uspto-grants-2015_04
특허 번호
US09018211B2

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