Dimethylformamide → 5-Methoxy-3-methyl-1-(3-methyl-3-nitro-butyl)-1,3-dihydro-benzimidazol-2-one

HRID 33392노트

반응식

HRID 33392 반응식
[H-].[Na+].[CH3:3][O:4][C:5]1[CH:15]=[CH:14][C:8]2[N:9]([CH3:13])[C:10](=[O:12])[NH:11][C:7]=2[CH:6]=1.ICC[CH2:19][C:20]([CH3:25])([N+:22]([O-:24])=[O:23])[CH3:21].[CH3:26]N(C=O)C>O>[CH3:3][O:4][C:5]1[CH:15]=[CH:14][C:8]2[N:9]([CH2:13][CH2:19][C:20]([CH3:25])([N+:22]([O-:24])=[O:23])[CH3:21])[C:10](=[O:12])[N:11]([CH3:26])[C:7]=2[CH:6]=1

참가 물질

6

반응물 4

HCID 6228Dimethylformamide2회HCID 24758Sodium hydrideHCID 99430631-Iodo-4-methyl-4-nitro-pentaneHCID 213212535-methoxy-1-methyl-1H-benzo[d]imidazol-2(3H)-one

생성물 1

HCID 671887485-Methoxy-3-methyl-1-(3-methyl-3-nitro-butyl)-1,3-dihydro-benzimidazol-2-one

시약·촉매·용매 1

HCID 962Water용매

실험 절차

1.1 g (28 mmol) 60% sodium hydride are added to 2.5 g (14 mmol) 5-methoxy-1-methyl-1,3-dihydro-benzimidazol-2-one in 30 mL DMF while being cooled with the ice bath. After 30 minutes a solution of 1-iodo-4-methyl-4-nitro-pentane in 20 mL DMF is piped in and the mixture is stirred overnight. It is diluted with water and extracted with ethyl acetate. The combined organic phases are washed with water, dried and evaporated down. The solid remaining is stirred with diethyl ether.

후처리

  1. extractionextracted with ethyl acetate
  2. washThe combined organic phases are washed with water
  3. customdried
  4. customevaporated down
  5. stirringThe solid remaining is stirred with diethyl ether

출처 및 근거

ORD 기록
ord-d35fe270f68d4d36ba671ea26580a9ec
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07429583B2

반응 노트

불러오는 중…