2-(Chloromethyl)-n-methylaniline hydrochloride → HCID 15027408、化合物

HRID 1090820ノート

反応式

HRID 1090820 の反応式
[SH:1][C:2]1[NH:6][C:5]2[CH2:7][CH2:8][CH2:9][CH2:10][C:4]=2[N:3]=1.Cl.[CH3:12][NH:13][C:14]1[CH:21]=[CH:20][CH:19]=[CH:18][C:15]=1[CH2:16]Cl>C(O)C>[CH3:12][NH:13][C:14]1[CH:21]=[CH:20][CH:19]=[CH:18][C:15]=1[CH2:16][S:1][C:2]1[NH:6][C:5]2[CH2:7][CH2:8][CH2:9][CH2:10][C:4]=2[N:3]=1

参加物

4

反応物 2

HCID 148394402-(Chloromethyl)-n-methylaniline hydrochlorideHCID 1785278154,5,6,7-tetrahydro-1H-benzimidazole-2-thiol

生成物 1

HCID 15027408HCID 15027408、化合物収率 53.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a suspension of 1.3 g (9 mmol) of 2-mercapto-4,5,6,7-tetrahydro-1H-benzimidazole in 20 ml of ethanol was added 1.35 g (7 mmol) of 2-methylaminobenzyl chloride hydrochloride for a period of 15 min. The solvent was distilled off, and the residue was shaken sufficiently with a combination of 1N aqueous sodium hydroxide and chloroform for performing extraction. The organic portion was taken out and then dried over anhydrous sodium sulfate. Chloroform was distilled off, and the residue was crystallized from ether/hexane to give 1.02 g of the desired compound as a pale brown crystalline product, yield 53%.

後処理

  1. distillationThe solvent was distilled off
  2. extractionextraction
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationChloroform was distilled off
  5. customthe residue was crystallized from ether/hexane

出典と根拠

ORDレコード
ord-84c8fc1fd55f48a6b03bcf4b7d80b76c
出典データセット
uspto-grants-1992_01
特許番号
US05082943

反応ノート

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