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

HRID 1594776노트

반응식

HRID 1594776 반응식
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

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 516892Sodium BicarbonateHCID 21706781HCID 21706781, 화합물

생성물 1

HCID 3168407-Hydroxy-6-methoxy-1-tetralone수율 97.9%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
25 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-42d556f317594c88847f0d8bf456bc3a
출처 데이터셋
uspto-grants-2001_09
특허 번호
US06284789B1

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