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

HRID 1729583

반응식

HRID 1729583 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-carbonitrile

시약·촉매·용매 1

HCID 1049Pyridine용매

반응 조건

온도
60 °C

실험 절차

Phosphorus oxychloride (POCl3) (42.4 ml - 0.44 mole) was added to a stirred and ice-cooled solution of IV (81.2 g - 0.4 mole) in pyridine (160 ml). The temperature reached 45° C. After this addition, the mixture was heated to 60° C. The reddish-brown oil was poured immediately in 1 kg of ice/water with stirring. The precipitate was filtered, washed with ice-cold water, and dried. The crude product was crystallized from pyridine (1.5 ml/g) and water (9 ml/g).

후처리

  1. customreached 45° C
  2. additionAfter this addition
  3. stirringwith stirring
  4. filtrationThe precipitate was filtered
  5. washwashed with ice-cold water
  6. customdried
  7. customThe crude product was crystallized from pyridine (1.5 ml/g) and water (9 ml/g)

출처 및 근거

ORD 기록
ord-f9fa9484b4744270ad3c1668120d0091
출처 데이터셋
uspto-grants-1976_11
특허 번호
US03989522

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