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

HRID 324917

반응식

HRID 324917 반응식
[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

참가 물질

6

반응물 3

HCID 7243O-PhenylenediamineHCID 84462-MethylbenzothiazoleHCID 5362487Sulfur

생성물 1

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

시약·촉매·용매 2

HCID 1049Pyridine용매2회HCID 57417360Sodium chloride; water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2d6cc20732844b04a3fbfb1784cb370e
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06221343B1

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