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

HRID 2179887

反応式

HRID 2179887 の反応式
[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

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-707090167f8a43f1941721a79a3024ae
出典データセット
uspto-grants-2005_05
特許番号
US06887867B2

関連ノート

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