Dimethylformamide → HCID 9799569、化合物

HRID 1595210ノート

反応式

HRID 1595210 の反応式
[OH:1][C:2]1[CH:3]=[C:4]2[O:24][C:23]([CH3:26])([CH3:25])[CH:22]=[CH:21][C:5]2=C2[C:15]=1[C:14](=[O:16])[C:13]1[CH:12]=[C:11]3[CH:17]=[CH:18][CH:19]=[CH:20][C:10]3=[CH:9]C=1N2.[H-].[Na+].S(OC)(O[CH3:33])(=O)=O.[CH3:36][N:37]([CH3:40])[CH:38]=O>>[CH3:33][O:1][C:2]1[CH:3]=[C:4]2[O:24][C:23]([CH3:26])([CH3:25])[CH:22]=[CH:21][C:5]2=[C:36]2[C:15]=1[C:14](=[O:16])[C:13]1[CH:12]=[C:11]3[CH:17]=[CH:18][CH:19]=[CH:20][C:10]3=[CH:9][C:38]=1[N:37]2[CH3:40]

参加物

5

反応物 4

HCID 6228DimethylformamideHCID 6497Dimethyl SulfateHCID 24758Sodium hydrideHCID 10665070HCID 10665070、化合物

生成物 1

HCID 9799569HCID 9799569、化合物

実験手順

To a solution of 0.5 g of the product of Example 1 in 20 ml of anhydrous dimethylformamide there are slowly added at 0° C., under an inert atmosphere, 0.16 g of sodium hydride and then, after 15 minutes, 0.65 ml of dimethyl sulphate (6 equivalents). After one hour, the reaction mixture is poured onto ice and then extracted with ethyl acetate. The organic phase is washed with an aqueous sodium hydroxide solution and subsequently dried over sodium sulphate and then evaporated in vacuo. Chromatography on silica gel (cyclohexane/acetone: 98/2) allows 0.42 g of the expected product to be isolated.

後処理

  1. waitAfter one hour
  2. additionthe reaction mixture is poured onto ice
  3. extractionextracted with ethyl acetate
  4. washThe organic phase is washed with an aqueous sodium hydroxide solution
  5. dry with materialsubsequently dried over sodium sulphate
  6. customevaporated in vacuo
  7. customto be isolated

出典と根拠

ORDレコード
ord-c0edfc83749541bbb4b588fcab740eb4
出典データセット
uspto-grants-2001_09
特許番号
US06288073B1

反応ノート

読み込み中…