Hydrochloric Acid → 2-Hydroxy-4,5-dimethoxybenzoic acid

HRID 1621066

反応式

HRID 1621066 の反応式
C[O:2][C:3]1[CH:11]=[C:10]([O:12][CH3:13])[C:9]([O:14][CH3:15])=[CH:8][C:4]=1[C:5]([OH:7])=[O:6].[Al](Cl)(Cl)Cl.O.O.O.O.O.O.[Na+].[Br-].Cl>CN(C)C=O.O>[OH:2][C:3]1[CH:11]=[C:10]([O:12][CH3:13])[C:9]([O:14][CH3:15])=[CH:8][C:4]=1[C:5]([OH:7])=[O:6]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 102762,4,5-Trimethoxybenzoic acidHCID 24564Aluminum chloride, hexahydrateHCID 253881Sodium Bromide

生成物 1

HCID 115646502-Hydroxy-4,5-dimethoxybenzoic acid収率 73.2%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
100 °C

実験手順

In 11 mL of dimethylformamide (DMF) were suspended 2.12 g of compound (1a), 4.82 g of AlCl3.6H2O, and 2.06 g of NaBr in a stream of argon, which was then heat stirred at 100° C. for 5 hours. The reaction mixture was allowed to stand to cool, to which 10.4 g of 35% hydrochloric acid was then added dropwise before adding 11 mL of water, followed by heat stirring at 70° C. for one hour. The precipitated crystal was collected by filtration and washed with water. The resultant crystal was dried under reduced pressure at 60° C. to provide 1.45 g of compound (2a) at a yield of 73%.

後処理

  1. temperaturewas then heat
  2. additionwas then added dropwise
  3. temperatureby heat
  4. stirringstirring at 70° C. for one hour
  5. filtrationThe precipitated crystal was collected by filtration
  6. washwashed with water
  7. customThe resultant crystal was dried under reduced pressure at 60° C.

出典と根拠

ORDレコード
ord-05ff0bb7d8c94884b8db9b5ce12897c4
出典データセット
uspto-grants-2014_07
特許番号
US08772528B2

関連ノート

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