Hydrochloric Acid → HCID 46935119、化合物

HRID 83099

反応式

HRID 83099 の反応式
[CH2:1]([O:8][C:9]1[CH:10]=[C:11]([OH:24])[C:12]2[C:13](=[O:23])[C:14]3[C:19]([O:20][C:21]=2[CH:22]=1)=[CH:18][CH:17]=[CH:16][CH:15]=3)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CI.[C:27]([O-])([O-])=O.[Cs+].[Cs+].Cl>O.C(Cl)Cl.CN(C=O)C>[CH2:1]([O:8][C:9]1[CH:10]=[C:11]([O:24][CH3:27])[C:12]2[C:13](=[O:23])[C:14]3[C:19]([O:20][C:21]=2[CH:22]=1)=[CH:18][CH:17]=[CH:16][CH:15]=3)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 6328Methyl iodideHCID 10796Cesium carbonateHCID 57412951-Hydroxy-3-phenylmethoxyxanthen-9-one

生成物 1

HCID 46935119HCID 46935119、化合物収率 97.9%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 6344Dichloromethane溶媒

実験手順

The compound (0.40 g, 1.26 mmol) prepared in Step 1 of Example 9, methyl iodide (535.68 mg, 3.77 mmol), and DMF (10 mL) were charged to a dry round-bottom flask, and Cs2CO3 (0.82 g, 2.52 mmol) was added thereto with stirring. The reaction mixture was stirred at 50° C. for 3 hours. After the reaction was completed, the reaction liquid was transferred to an Erlenmeyer flask, and the reaction container was washed with methylene chloride. The reaction contents were combined and acidified with 2M-HCl on ice water. After being warmed to room temperature, CH2Cl2 (20 mL) and water (10 mL) were added and the reaction liquid was repeatedly extracted with methylene chloride. The organic layer was combined, washed with water and brine, and then dried over anhydrous Na2SO4. The solvent was removed under reduced pressure. Ethanol was added to the resulting sludge-like material, followed by trituration, and the resulting solid was filtered to give a white solid compound (0.41 g, 97.3%).

後処理

  1. stirringThe reaction mixture was stirred at 50° C. for 3 hours
  2. customthe reaction liquid
  3. washthe reaction container was washed with methylene chloride
  4. customThe reaction contents
  5. customthe reaction liquid
  6. extractionwas repeatedly extracted with methylene chloride
  7. washwashed with water and brine
  8. dry with materialdried over anhydrous Na2SO4
  9. customThe solvent was removed under reduced pressure
  10. additionEthanol was added to the resulting sludge-like material
  11. filtrationthe resulting solid was filtered

出典と根拠

ORDレコード
ord-3354b3151e88451098da4bc66ad6e990
出典データセット
uspto-grants-2014_09
特許番号
US08846749B2

関連ノート

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