Acetone → 6-Bromo-2,2-dimethyl-4H-benzo[d][1,3]dioxine

HRID 490991

反応式

HRID 490991 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([OH:10])=[C:6]([CH:9]=1)[CH2:7][OH:8].[CH3:11][C:12]([CH3:14])=O.[OH-].[Na+].C(OCC)C>COC(OC)(C)C.[Cl-].[Zn+2].[Cl-]>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[O:10][C:12]([CH3:14])([CH3:11])[O:8][CH2:7][C:6]=2[CH:9]=1

参加物

7

反応物 4

HCID 180AcetoneHCID 3283Diethyl EtherHCID 14798Sodium HydroxideHCID 753425-Bromo-2-hydroxybenzyl alcohol

生成物 1

HCID 145203386-Bromo-2,2-dimethyl-4H-benzo[d][1,3]dioxine

試薬・触媒・溶媒 2

HCID 3007855Zincchloride触媒HCID 64952,2-Dimethoxypropane溶媒

実験手順

To 5-bromo-2-hydroxybenzyl alcohol (93 g, 0.46 mol, available from Sigma-Aldrich) in 2.0 L of 2,2-dimethoxypropane was added 700 mL of acetone, followed by zinc chloride (170 g). After stirring for 18 hours, 1.0 M aqueous sodium hydroxide was added until the aqueous phase was basic. Diethyl ether (1.5 L) was added to the slurry and the organic phase was decanted into a separatory funnel. The organic phase was washed with brine, dried over Na2SO4, filtered and concentrated under reduced pressure to give the title compound as an oil.

後処理

  1. customthe organic phase was decanted into a separatory funnel
  2. washThe organic phase was washed with brine
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-24c3fb42e0934fb991e8732fbc4a985d
出典データセット
uspto-grants-2009_05
特許番号
US07528253B2

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