Diisopropyl Ether → 5-Methylbenzimidazolone

HRID 1503225노트

반응식

HRID 1503225 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([NH2:8])=[C:4]([NH2:9])[CH:3]=1.[C:10](N1C=CN=C1)(N1C=CN=C1)=[O:11].C(OC(C)C)(C)C>O1CCCC1.ClCCl>[CH3:1][C:2]1[CH:7]=[CH:6][C:5]2[NH:8][C:10](=[O:11])[NH:9][C:4]=2[CH:3]=1

참가 물질

6

반응물 3

HCID 7914Diisopropyl EtherHCID 103323,4-DiaminotolueneHCID 682631,1'-Carbonyldiimidazole

생성물 1

HCID 2231345-Methylbenzimidazolone수율 81.1%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 4-methyl-1,2-phenylenediamine (1) (25 g) in tetrahydrofuran (375 mL) was added dropwise a solution of 1,1′-carbonyldiimidazole (36.5 g) in dichloromethane (375 mL). After stirring at room temperature for 6.5 hr, diisopropylether (375 mL) was added to the reaction mixture. After stirring at room temperature, the resulting precipitate was collected by filtration. The precipitate was washed with diisopropyl ether, and dried under reduced pressure to give 5-methyl-1,3-dihydrobenzimidazol-2-one (2) (24.6 g).

후처리

  1. stirringAfter stirring at room temperature
  2. filtrationthe resulting precipitate was collected by filtration
  3. washThe precipitate was washed with diisopropyl ether
  4. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-5d4a4d46e4d341b2ad72b1f0468b94d1
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09212169B2

반응 노트

불러오는 중…