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

HRID 1983208ノート

反応式

HRID 1983208 の反応式
[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]

参加物

4

反応物 2

HCID 23668300Sodium 4-cyanobenzenesulfinateHCID 67174878HCID 67174878、化合物

生成物 1

HCID 220550573-Ethyl-2-methylbenzoxazolium 4-Cyanobenzenesulfinate収率 46.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ef5322217c2847908cf5b2c6e9c9a8b7
出典データセット
uspto-grants-2009_06
特許番号
US07541389B2

反応ノート

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