2-(Chloromethyl)-n-methylaniline hydrochloride → 2-(2-Methylaminobenzylthio)imidazole

HRID 1646699ノート

反応式

HRID 1646699 の反応式
[SH:1][C:2]1[NH:3][CH:4]=[CH:5][N:6]=1.Cl.[CH3:8][NH:9][C:10]1[CH:17]=[CH:16][CH:15]=[CH:14][C:11]=1[CH2:12]Cl>C(O)C>[CH3:8][NH:9][C:10]1[CH:17]=[CH:16][CH:15]=[CH:14][C:11]=1[CH2:12][S:1][C:2]1[NH:3][CH:4]=[CH:5][N:6]=1

参加物

4

反応物 2

HCID 148394402-(Chloromethyl)-n-methylaniline hydrochlorideHCID 178527877HCID 178527877、化合物

生成物 1

HCID 150274142-(2-Methylaminobenzylthio)imidazole収率 65.5%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 693 mg (6.9 mmol) of 2-mercapto-imidazole in 26 ml of ethanol was added 1.33 g (6.9 mmol) of 2-methylaminobenzyl chloride hydrochloride, and the mixture was stirred for 15 min. at room temperature. Ethanol was distilled off under reduced pressure. The residue was made alkaline by addition of saturated aqueous sodium hydrogencarbonate and then to the alkaline solution was added 20 ml of water to precipitate a crystalline product. The product was collected by filtration and washed successively with two portions of water and each one portion of chilled ethanol and ether to give 990 mg of the desired compound as a white crystalline powder, yield 65.5%.

後処理

  1. distillationEthanol was distilled off under reduced pressure
  2. additionby addition of saturated aqueous sodium hydrogencarbonate
  3. additionto the alkaline solution was added 20 ml of water
  4. customto precipitate a crystalline product
  5. filtrationThe product was collected by filtration
  6. washwashed successively with two portions of water

出典と根拠

ORDレコード
ord-3672da3472ae42ecbb3c04c2f5a0484a
出典データセット
uspto-grants-1993_01
特許番号
US05180836

反応ノート

読み込み中…