Dimethylformamide → HCID 9799569, 화합물

HRID 1595210노트

반응식

HRID 1595210 반응식
[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]

참가 물질

5

반응물 4

HCID 6228DimethylformamideHCID 6497Dimethyl SulfateHCID 24758Sodium hydrideHCID 10665070HCID 10665070, 화합물

생성물 1

HCID 9799569HCID 9799569, 화합물

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c0edfc83749541bbb4b588fcab740eb4
출처 데이터셋
uspto-grants-2001_09
특허 번호
US06288073B1

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