Dimethylformamide → HCID 9799569、化合物

HRID 478684ノート

反応式

HRID 478684 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 obtained in Step B 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 1 hour, the reaction mixture is hydrolysed using ice and is then extracted with ethyl acetate. After washing the organic phase with aqueous sodium hydroxide solution, it is dried over sodium sulphate and then evaporated in vacuo. Chromatography over silica gel (cyclohexane/acetone: 98/2) allows 0.42 g of the expected product to be obtained. Melting point: 188° C.

後処理

  1. waitAfter 1 hour
  2. extractionis then extracted with ethyl acetate
  3. washAfter washing the organic phase with aqueous sodium hydroxide solution, it
  4. dry with materialis dried over sodium sulphate
  5. customevaporated in vacuo
  6. customto be obtained

出典と根拠

ORDレコード
ord-5f6fa2158dde48a69058e58af666f5fb
出典データセット
uspto-grants-2003_11
特許番号
US06642248B2

反応ノート

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