2-(Chloromethyl)-n-methylaniline hydrochloride → HCID 15027408, 화합물

HRID 1646695노트

반응식

HRID 1646695 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 15027408HCID 15027408, 화합물수율 53.3%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-f8a1dbda0e464190b7ba9f5c08f3b368
출처 데이터셋
uspto-grants-1993_01
특허 번호
US05180836

반응 노트

불러오는 중…