Hydrochloric Acid → 7-Hydroxy-6-methoxy-1-tetralone

HRID 1594776ノート

反応式

HRID 1594776 の反応式
O.C(=O)(O)[O-].[Na+].C([O:10][C:11]1[CH:20]=[C:19]2[C:14]([CH2:15][CH2:16][CH2:17][C:18]2=[O:21])=[CH:13][C:12]=1[O:22][CH3:23])(=O)C.Cl>CO>[CH3:23][O:22][C:12]1[CH:13]=[C:14]2[C:19](=[CH:20][C:11]=1[OH:10])[C:18](=[O:21])[CH2:17][CH2:16][CH2:15]2

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 516892Sodium BicarbonateHCID 21706781HCID 21706781、化合物

生成物 1

HCID 3168407-Hydroxy-6-methoxy-1-tetralone収率 97.9%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
25 °C

実験手順

3.5 mL of water and then 3.5 mL of saturated aqueous sodium bicarbonate was added to 117 mg of 7-acetoxy-6-methoxytetralin- 1-one dissolved in 7 mL of methanol. The resulting solution was stirred under nitrogen at 25° C. for 17 hours. Thereafter the solution was acidified with aqueous hydrogen chloride and extracted five times with 6 mL portions of methylene chloride. The combined methylene chloride extracts were washed once with brine and dried over anhydrous magnesium sulfate. The dried extract was separated by filtration and the methylene chloride was removed from the filtrate by evaporation at reduced atmospheric pressure and gave 94 mg of 6-methoxy-7-hydroxytetralin-1-one having m.p. 151-152° C.

後処理

  1. extractionextracted five times with 6 mL portions of methylene chloride
  2. washThe combined methylene chloride extracts were washed once with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. extractionThe dried extract
  5. customwas separated by filtration
  6. customthe methylene chloride was removed from the filtrate by evaporation at reduced atmospheric pressure

出典と根拠

ORDレコード
ord-42d556f317594c88847f0d8bf456bc3a
出典データセット
uspto-grants-2001_09
特許番号
US06284789B1

反応ノート

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