2-(Chloromethyl)aniline hydrochloride → HCID 178488113, 화합물

HRID 1071535노트

반응식

HRID 1071535 반응식
[SH:1][C:2]1[NH:3][C:4]2[CH:10]=[C:9]([O:11][CH3:12])[CH:8]=[CH:7][C:5]=2[N:6]=1.Cl.Cl[CH2:15][C:16]1[CH:22]=[CH:21][CH:20]=[CH:19][C:17]=1[NH2:18]>C(O)(C)C>[CH3:12][O:11][C:9]1[CH:8]=[CH:7][C:5]2[NH:6][C:2]([S:1][CH2:15][C:16]3[CH:22]=[CH:21][CH:20]=[CH:19][C:17]=3[NH2:18])=[N:3][C:4]=2[CH:10]=1

참가 물질

4

반응물 2

HCID 123879412-(Chloromethyl)aniline hydrochlorideHCID 178488032HCID 178488032, 화합물

생성물 1

HCID 178488113HCID 178488113, 화합물수율 19.5%

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

The title compound was prepared by the method of Example 1 using 1.68 g (9.33 mmole) of 2-mercapto-5-methoxybenzimidazole instead of 2-mercaptobenzimidazole and 1.99 g (11.2 mmole) of 2-(chloromethyl)aniline hydrochloride instead of 2-(chloromethyl)-N,N-dimethylaniline in 250 ml of isopropyl alcohol. The basic extraction used 5% sodium hydroxide instead of sodium carbonate. Chromatography on silica gel, followed by crystallization from diethylether, gave 520 mg of pure title compound: m.p. 140-142° C. Analysis. Calc'd. for C15H15N3OS: C, 63.14; H, 5.30; N,14.73; S, 11.23. Found: C, 63.44; H, 5.42; N, 14.43; S, 11.07.

후처리

  1. extractionThe basic extraction
  2. customChromatography on silica gel, followed by crystallization from diethylether

출처 및 근거

ORD 기록
ord-05271fab702148c1b8037593c7a394bf
출처 데이터셋
uspto-grants-2005_06
특허 번호
US06906078B2

반응 노트

불러오는 중…