Hydrochloric Acid → 2-[(4-Bromophenyl)thio]-N,N-dimethylethanamine

HRID 1111146노트

반응식

HRID 1111146 반응식
Cl[CH2:2][CH2:3][N:4]([CH3:6])[CH3:5].Cl.[OH-].[Na+].[Br:10][C:11]1[CH:16]=[CH:15][C:14]([SH:17])=[CH:13][CH:12]=1>C(O)C>[CH3:5][N:4]([CH2:3][CH2:2][S:17][C:14]1[CH:15]=[CH:16][C:11]([Br:10])=[CH:12][CH:13]=1)[CH3:6]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 79012-Chloro-N,N-dimethylethylamineHCID 14798Sodium Hydroxide3회HCID 660494-Bromothiophenol

생성물 1

HCID 248380762-[(4-Bromophenyl)thio]-N,N-dimethylethanamine수율 86%

시약·촉매·용매 1

HCID 702Ethanol용매3회

실험 절차

A solution of 23.5 g of chloroethyldimethylamine.HCl in 75 ml of ethanol was added to 160 ml of sodium hydroxide solution formed by dissolving 20 g of sodium hydroxide pastilles in 500 ml of ethanol. A solution of 30 g of 4-bromothiophenol in 100 ml of ethanol was added to 160 ml of the said sodium hydroxide solution and the first solution was added thereto over 2 minutes at 20° C. The mixture was refluxed for 3 hours and was evaporated to dryness. Water was added to the residue and the mixture was extracted with methylene chloride. The organic phase was washed with aqueous 0.1N sodium hydroxide solution, then with water, dried and evaporated to dryness. The residue was distilled to obtain 35.5 g of 4-(N,N-dimethylaminoethylthio)-bromobenzene boiling at 110° C. at 0.1 mm Hg.

후처리

  1. customformed
  2. additionthe first solution was added
  3. temperatureThe mixture was refluxed for 3 hours
  4. customwas evaporated to dryness
  5. additionWater was added to the residue
  6. extractionthe mixture was extracted with methylene chloride
  7. washThe organic phase was washed with aqueous 0.1N sodium hydroxide solution
  8. dry with materialwith water, dried
  9. customevaporated to dryness
  10. distillationThe residue was distilled

출처 및 근거

ORD 기록
ord-1c451b5d1f93439ba43278a1a1ac3096
출처 데이터셋
uspto-grants-1990_12
특허 번호
US04978657

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