N-Iodosuccinimide → HCID 59155826, 화합물

HRID 1662884노트

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HRID 1662884 반응식
[CH2:1]([O:3][P:4]([C:9]1[CH:13]=[CH:12][S:11][CH:10]=1)([O:6][CH2:7][CH3:8])=[O:5])[CH3:2].[I:14]N1C(=O)CCC1=O.P([O-])([O-])(O)=O.[Na+].[Na+].P([O-])(O)(O)=O.[Na+]>C(Cl)(Cl)Cl.C(O)(=O)C>[I:14][C:12]1[S:11][CH:10]=[C:9]([P:4]([O:6][CH2:7][CH3:8])([O:3][CH2:1][CH3:2])=[O:5])[CH:13]=1

참가 물질

6

반응물 3

HCID 120273N-IodosuccinimideHCID 153633033-(Diethoxyphosphoryl)thiopheneHCID 86630341Sodium phosphate (Na3(PO4)2)

생성물 1

HCID 59155826HCID 59155826, 화합물수율 73%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 6212Chloroform용매

실험 절차

In 5 ml of a mixed solvent of chloroform:acetic acid=1:1, 0.1101 g (0.5 mmols) of 3-(diethoxyphosphoryl)thiophene was dissolved, to which 0.2362 g (1.05 mmols) of commercially available N-iodosuccinimide was added at room temperature. Thereafter, the reaction mixture was stirred at room temperature for 4 days. After the reaction, a disodium hydrogen phosphate/sodium dihydrogen phosphate buffer solution, adjusted to pH=7, was added, followed by extraction with chloroform. The organic phase was washed with a 0.2N sodium hydroxide aqueous solution and dried over anhydrous sodium sulfate. The solvent was removed, and the resulting crude product was purified with a PTLC plate (developed with ethyl acetate:hexane 1:1) to obtain the specified substance in the form of a yellow oil at a yield of 0.1263 g (yield: 73%). The thus obtained substance was used as it is for reaction in Example 12(9).

후처리

  1. additionwas added at room temperature
  2. customAfter the reaction
  3. additionwas added
  4. extractionfollowed by extraction with chloroform
  5. washThe organic phase was washed with a 0.2N sodium hydroxide aqueous solution
  6. dry with materialdried over anhydrous sodium sulfate
  7. customThe solvent was removed
  8. customthe resulting crude product was purified with a PTLC plate (developed with ethyl acetate:hexane 1:1)
  9. customto obtain the specified substance in the form of a yellow oil at a yield of 0.1263 g (yield: 73%)
  10. customis for reaction in Example 12(9)

출처 및 근거

ORD 기록
ord-e62db8f22eda466ab3e1fcec2b31b9bd
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08030438B2

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