Sodium Hydroxide → 2-[(4-Bromophenyl)thio]-N,N-dimethylethanamine

HRID 979796ノート

反応式

HRID 979796 の反応式
Cl.Cl[CH2:3][CH2:4][N:5]([CH3:7])[CH3:6].[OH-].[Na+].[Br:10][C:11]1[CH:16]=[CH:15][C:14]([SH:17])=[CH:13][CH:12]=1>C(O)C>[CH3:6][N:5]([CH2:4][CH2:3][S:17][C:14]1[CH:15]=[CH:16][C:11]([Br:10])=[CH:12][CH:13]=1)[CH3:7]

参加物

5

反応物 3

HCID 14798Sodium Hydroxide3 回HCID 660494-BromothiophenolHCID 11636816N,N-Dimethylaminoethyl chloride hydrochloride

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒3 回

実験手順

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 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.

後処理

  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 1N sodium hydroxide solution
  8. dry with materialwith water, dried
  9. customevaporated to dryness
  10. distillationThe residue was distilled

出典と根拠

ORDレコード
ord-d63427d8ba7149b7aab966e228185fc2
出典データセット
uspto-grants-1987_01
特許番号
US04634695

反応ノート

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