Sodium Hydroxide → HCID 19996498, 화합물

HRID 2248439노트

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HRID 2248439 반응식
[CH3:1][C:2]1[C:10]2[N:9]=[C:8]([SH:11])[NH:7][C:6]=2[CH:5]=[C:4]([CH3:12])[C:3]=1[O:13][CH3:14].[OH-].[Na+].Cl.[CH3:18][C:19]1[C:20]([CH2:26]Cl)=[N:21][CH:22]=[CH:23][C:24]=1[CH3:25]>CO.O>[CH3:1][C:2]1[C:10]2[N:9]=[C:8]([S:11][CH2:26][C:20]3[C:19]([CH3:18])=[C:24]([CH3:25])[CH:23]=[CH:22][N:21]=3)[NH:7][C:6]=2[CH:5]=[C:4]([CH3:12])[C:3]=1[O:13][CH3:14]

참가 물질

6

반응물 3

HCID 14798Sodium Hydroxide2회HCID 199964993,4-Dimethyl-2-chloromethylpyridine hydrochlorideHCID 178489086HCID 178489086, 화합물

생성물 1

HCID 19996498HCID 19996498, 화합물수율 67.2%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매2회

실험 절차

To 4,6-dimethyl-5-methoxy-2-mercapto-1H-benzimidazole (1.04 g, 0.0050 mol) in methanol (50 ml) were added (in the following order) NaOH (0.2 g, 0.0050 mol) dissolved in water (2 ml) and 3,4-dimethyl-2-chloromethylpyridine hydrochloride (0.96 g, 0.0050 mol). The mixture was heated until reflux. NaOH (0.2 g, 0.0050 mol) dissolved in water (2 ml) was added dropwise and then the reflux was continued for 3 hours. The mixture was poured on ice-water (200 ml). Filtration and recrystallization from CH3CN gave the desired product (1.1 g, 67%). NMR data for the final product is given below.

후처리

  1. temperatureThe mixture was heated
  2. temperatureuntil reflux
  3. additionwas added dropwise
  4. additionThe mixture was poured on ice-water (200 ml)
  5. filtrationFiltration and recrystallization from CH3CN

출처 및 근거

ORD 기록
ord-c2f88b031b4a48d5ba58e4a47a9dae02
출처 데이터셋
uspto-grants-1991_08
특허 번호
US05039806

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