O-Phenylenediamine → 2-(1H-Benzimidazol-2-yl)-1,3-benzothiazole

HRID 324917

反応式

HRID 324917 の反応式
[CH3:1][C:2]1[S:3][C:4]2[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=1.[C:11]1([NH2:18])[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[NH2:17].[S]>N1C=CC=CC=1.[Cl-].[Na+].O>[NH:17]1[C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=2[N:18]=[C:1]1[C:2]1[S:3][C:4]2[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=1

参加物

6

反応物 3

HCID 7243O-PhenylenediamineHCID 84462-MethylbenzothiazoleHCID 5362487Sulfur

生成物 1

HCID 3738782-(1H-Benzimidazol-2-yl)-1,3-benzothiazole収率 13.7%

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒2 回HCID 57417360Sodium chloride; water溶媒

実験手順

The heterogeneous mixture consisting of methylbenzothiazole (59.6 g, 0.4 mol), ortho-phenylenediamine (43.2 g, 0.4 mol) and sulfur (38.4 g, 1.2 mol) in 300 ml of pyridine was heated at the reflux point of pyridine for 22 hours. The reaction mixture was cooled and poured into a solution of brine. After extraction with ethyl acetate, washing of the organic phase 3 times with water, drying over sodium sulfate and concentration of the solvent under vacuum, the solid obtained was washed with acetone. After drying, 2-(1H-benzimidazol-2-yl)benzothiazole (13.8 g, yield: 13%) was obtained in the form of a yellow solid.

後処理

  1. temperatureThe reaction mixture was cooled
  2. extractionAfter extraction with ethyl acetate
  3. washwashing of the organic phase 3 times with water
  4. dry with materialdrying over sodium sulfate and concentration of the solvent under vacuum
  5. customthe solid obtained
  6. washwas washed with acetone
  7. customAfter drying

出典と根拠

ORDレコード
ord-2d6cc20732844b04a3fbfb1784cb370e
出典データセット
uspto-grants-2001_04
特許番号
US06221343B1

関連ノート

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