Sodium 4-cyanobenzenesulfinate → 3-Ethyl-2-methylbenzoxazolium 4-Cyanobenzenesulfinate

HRID 1983208노트

반응식

HRID 1983208 반응식
[Cl-].[CH2:2]([N+:4]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[O:6][C:5]=1[CH3:13])[CH3:3].[C:14]([C:16]1[CH:21]=[CH:20][C:19]([S:22]([O-:24])=[O:23])=[CH:18][CH:17]=1)#[N:15].[Na+]>C(O)C>[C:14]([C:16]1[CH:17]=[CH:18][C:19]([S:22]([O-:24])=[O:23])=[CH:20][CH:21]=1)#[N:15].[CH2:2]([N+:4]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[O:6][C:5]=1[CH3:13])[CH3:3]

참가 물질

4

반응물 2

HCID 23668300Sodium 4-cyanobenzenesulfinateHCID 67174878HCID 67174878, 화합물

생성물 1

HCID 220550573-Ethyl-2-methylbenzoxazolium 4-Cyanobenzenesulfinate수율 46.1%

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

A solution of 3-ethyl-2-methylbenzoxazolium chloride (0.73 g) in ethanol (20 mL) was added to an Erlenmeyer flask containing a magnetically stirred boiling solution of sodium 4-cyanobenzenesulfinate (0.1 g) in anhydrous ethanol (20 mL). The mixture was allowed to cool to room temperature and was then further cooled in an ice bath. The mixture was filtered and the filtrate was concentrated to dryness using a rotary evaporator. The residue was mixed with deionized water and this mixture was extracted with ethyl acetate (2×20 mL). The combined organic extracts were concentrated to dryness using a rotary evaporator. The resultant solid was then dissolved in methylene chloride, filtered and evaporated to dryness using a rotary evaporator to afford 0.08 g of product.

후처리

  1. additioncontaining
  2. temperaturewas then further cooled in an ice bath
  3. filtrationThe mixture was filtered
  4. concentrationthe filtrate was concentrated to dryness
  5. customa rotary evaporator
  6. additionThe residue was mixed with deionized water
  7. extractionthis mixture was extracted with ethyl acetate (2×20 mL)
  8. concentrationThe combined organic extracts were concentrated to dryness
  9. customa rotary evaporator
  10. dissolutionThe resultant solid was then dissolved in methylene chloride
  11. filtrationfiltered
  12. customevaporated to dryness
  13. customa rotary evaporator

출처 및 근거

ORD 기록
ord-ef5322217c2847908cf5b2c6e9c9a8b7
출처 데이터셋
uspto-grants-2009_06
특허 번호
US07541389B2

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