Phosphorus oxychloride → 1-Ethyl-2-methyl-1H-benzimidazole-5-carbonitrile

HRID 461297

반응식

HRID 461297 반응식
P(Cl)(Cl)(Cl)=O.[CH2:6]([N:8]1[C:12]2[CH:13]=[CH:14][C:15]([C:17](=O)[NH2:18])=[CH:16][C:11]=2[N:10]=[C:9]1[CH3:20])[CH3:7]>N1C=CC=CC=1>[CH2:6]([N:8]1[C:12]2[CH:13]=[CH:14][C:15]([C:17]#[N:18])=[CH:16][C:11]=2[N:10]=[C:9]1[CH3:20])[CH3:7]

참가 물질

4

반응물 2

HCID 24813Phosphorus oxychlorideHCID 292579Mls000756290

생성물 1

HCID 7223851-Ethyl-2-methyl-1H-benzimidazole-5-carbonitrile수율 61%

시약·촉매·용매 1

HCID 1049Pyridine용매

반응 조건

온도
60 °C

실험 절차

42.4 ml (0.44 mole) of phosphorus oxychloride were added to a stirred and ice-cooled solution of 81.2 g (0.4 mole) of compound IV in 160 ml of pyridine. The temperature reached 45° C. Thereupon the mixture was heated to 60° C. The reddish-brown oil obtained was poored immediately in 1 kg of an ice-water mixture with stirring. The precipitate was filtered, washed with ice-cold water and dried. The crude product obtained was crystallized from pyridine (1.5 ml/g) and water (9 mg/g). Melting point: 162° C. Yield: 61% (452 g).

후처리

  1. customreached 45° C
  2. customThe reddish-brown oil obtained
  3. stirringwith stirring
  4. filtrationThe precipitate was filtered
  5. washwashed with ice-cold water
  6. customdried

출처 및 근거

ORD 기록
ord-478948bf574d48a0a41448557b7bfbd4
출처 데이터셋
uspto-grants-1977_12
특허 번호
US04062682

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