Sodium Hydroxide → HCID 19996498、化合物

HRID 2248439ノート

反応式

HRID 2248439 の反応式
[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]

参加物

6

反応物 3

HCID 14798Sodium Hydroxide2 回HCID 199964993,4-Dimethyl-2-chloromethylpyridine hydrochlorideHCID 178489086HCID 178489086、化合物

生成物 1

HCID 19996498HCID 19996498、化合物収率 67.2%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c2f88b031b4a48d5ba58e4a47a9dae02
出典データセット
uspto-grants-1991_08
特許番号
US05039806

反応ノート

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