Triphosgene → 4-Nitro-1H-benzo[d]imidazol-2(3H)-one

HRID 1696345노트

반응식

HRID 1696345 반응식
ClC(Cl)(O[C:5](=[O:11])OC(Cl)(Cl)Cl)Cl.[N+:13]([C:16]1[C:17]([NH2:23])=[C:18]([NH2:22])[CH:19]=[CH:20][CH:21]=1)([O-:15])=[O:14]>CC#N>[N+:13]([C:16]1[C:17]2[NH:23][C:5](=[O:11])[NH:22][C:18]=2[CH:19]=[CH:20][CH:21]=1)([O-:15])=[O:14]

참가 물질

4

반응물 2

HCID 94429TriphosgeneHCID 43595253-Nitro-1,2-phenylenediamine

생성물 1

HCID 41498284-Nitro-1H-benzo[d]imidazol-2(3H)-one

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

Triphosgene (56 g, 188.8 mol) was added portionwise over 15 min to a solution of 3-nitro-1,2-phenylenediamine (25.5 g, 167 mol) in CH3CN (400 mL) at 0° C. and the mixture was allowed to warm to ambient temperature after 30 min. The reaction was concentrated in vacuo, diluted with toluene (100 mL) and the solid precipitate was collected by filtration to give the title compound. MS: m/z=180 (M+1).

후처리

  1. concentrationThe reaction was concentrated in vacuo
  2. additiondiluted with toluene (100 mL)
  3. filtrationthe solid precipitate was collected by filtration

출처 및 근거

ORD 기록
ord-525421729959483d9dc8801edf302430
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08163752B2

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