Hydrochloric Acid → Methyl 4-acetoxy-3-bromobenzoate

HRID 41172ノート

反応式

HRID 41172 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH:9]=[CH:10][C:11]=1[OH:12])[C:5]([O:7][CH3:8])=[O:6].N1C=CC=CC=1.[C:19](Cl)(=[O:21])[CH3:20].Cl>C(Cl)Cl.O>[C:19]([O:12][C:11]1[CH:10]=[CH:9][C:4]([C:5]([O:7][CH3:8])=[O:6])=[CH:3][C:2]=1[Br:1])(=[O:21])[CH3:20]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 6367Acetyl chlorideHCID 4778958Methyl 3-bromo-4-hydroxybenzoate

生成物 1

HCID 45037033Methyl 4-acetoxy-3-bromobenzoate収率 94.1%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

To a stirred suspension of methyl 3-bromo-4-hydroxybenzoate (270 g, 1168 mmol) in DCM (1.5 L) was added pyridine (150 mL). Acetyl chloride (87 mL, 1227 mmol) was then added dropwise at room temperature and under nitrogen. The mixture was left to stir for 2 h at room temperature. Water (1 L) was then added followed by HCl 2N until pH 1. The organic layer was then washed with water, brine, dried over MgSO4, filtered and evaporated to dryness to afford methyl 4-acetoxy-3-bromobenzoate (300 g, 94%) as a white powder.

後処理

  1. waitThe mixture was left
  2. washThe organic layer was then washed with water, brine
  3. dry with materialdried over MgSO4
  4. filtrationfiltered
  5. customevaporated to dryness

出典と根拠

ORDレコード
ord-b1db9f58bdde4b459567629dac1f7cd7
出典データセット
uspto-grants-2013_09
特許番号
US08530470B2

反応ノート

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