Sodium Hydroxide → HCID 178492290、化合物

HRID 1583999ノート

反応式

HRID 1583999 の反応式
[OH-].[Na+].[SH:3][C:4]1[NH:8][C:7]2[CH:9]=[CH:10][C:11]([O:13][C:14]([F:17])([F:16])[F:15])=[CH:12][C:6]=2[N:5]=1.Cl.Cl[CH2:20][C:21]1[C:26]([CH3:27])=[C:25]([O:28][CH3:29])[C:24]([CH3:30])=[CH:23][N:22]=1>C(O)C>[CH3:29][O:28][C:25]1[C:24]([CH3:30])=[CH:23][N:22]=[C:21]([CH2:20][S:3][C:4]2[NH:8][C:7]3[CH:9]=[CH:10][C:11]([O:13][C:14]([F:17])([F:15])[F:16])=[CH:12][C:6]=3[N:5]=2)[C:26]=1[CH3:27]

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 116942582-(Chloromethyl)-3,5-dimethyl-4-methoxypyridine hydrochlorideHCID 178506357HCID 178506357、化合物

生成物 1

HCID 178492290HCID 178492290、化合物収率 79%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

5 ml of 4M sodium hydroxide solution are added dropwise to a mixture of 2.34 g of 2-mercapto-5-trifluromethoxy-1H-benzimidazole and 2.2 g of 2-chloromethyl-4-methoxy-3,5-dimethylpyridine hydrochloride in 50 ml of ethanol at room temperature and the mixture is stirred overnight at room temperature. The solvent is distilled off in vacuo, water is added, the mixture is extracted with ethyl acetate, the solution is dried and 4.3 g (95%) of the dihydrochloride of the title compound are precipitated with 4M hydrogen chloride in ether. The salt is dissolved in water and the base is precipitated with dilute sodium carbonate solution at pH 8 and recrystallized from diisopropyl ether. 3.0 g (78%) of the title compound of m.p. 152°-154° C. are obtained.

後処理

  1. distillationThe solvent is distilled off in vacuo, water
  2. additionis added
  3. extractionthe mixture is extracted with ethyl acetate
  4. customthe solution is dried
  5. custom4.3 g (95%) of the dihydrochloride of the title compound are precipitated with 4M hydrogen chloride in ether
  6. dissolutionThe salt is dissolved in water
  7. customthe base is precipitated with dilute sodium carbonate solution at pH 8
  8. customrecrystallized from diisopropyl ether

出典と根拠

ORDレコード
ord-e3e2899740034d2b85f014d4e8eb3013
出典データセット
uspto-grants-1985_11
特許番号
US04555518

反応ノート

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