Hydrochloric Acid → 1-Hydroxy-3-methyl-1-(4-nitrophenyl)-6-methoxyisochroman

HRID 2179887

반응식

HRID 2179887 반응식
[CH3:1][CH:2]1[CH2:11][C:10]2[C:5](=[CH:6][CH:7]=[C:8]([O:12][CH3:13])[CH:9]=2)[CH:4]([C:14]2[CH:19]=[CH:18][C:17]([N+:20]([O-:22])=[O:21])=[CH:16][CH:15]=2)[O:3]1.[OH-:23].[Na+].Cl>CS(C)=O.CN(C=O)C>[OH:23][C:4]1([C:14]2[CH:19]=[CH:18][C:17]([N+:20]([O-:22])=[O:21])=[CH:16][CH:15]=2)[C:5]2[C:10](=[CH:9][C:8]([O:12][CH3:13])=[CH:7][CH:6]=2)[CH2:11][CH:2]([CH3:1])[O:3]1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 224889743-Methyl-1-(4-nitrophenyl)-6-methoxyisochroman

생성물 1

HCID 224889711-Hydroxy-3-methyl-1-(4-nitrophenyl)-6-methoxyisochroman

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 6228Dimethylformamide용매

실험 절차

A solution of 3 (1.3 g) in 4 ml of DMSO and 24 ml of DMF was cooled to 8-12° C. and air was passed through the mixture. To the solution was added 1.2 ml of 50% aqueous sodium hydroxide in one portion and the resulting mixture was stirred for 5 hours. HCl (1 N) was added, and extracted with ethyl acetate three times. The combined organic phase was washed with water in order to remove DMF, dried over Na2SO4. Removal of the solvent afforded syrup crude product (1.6 g), which was used directly for the next step.

후처리

  1. extractionextracted with ethyl acetate three times
  2. washThe combined organic phase was washed with water in order
  3. customto remove DMF
  4. dry with materialdried over Na2SO4
  5. customRemoval of the solvent

출처 및 근거

ORD 기록
ord-707090167f8a43f1941721a79a3024ae
출처 데이터셋
uspto-grants-2005_05
특허 번호
US06887867B2

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