Dimethylamine → Evt-201

HRID 651574노트

반응식

HRID 651574 반응식
[Cl:1][C:2]1[C:7]2[C:8](=[O:24])[N:9]([CH3:23])[CH2:10][C:11]3[N:12]([CH:13]=[N:14][C:15]=3[C:16]3[N:20]=[C:19]([CH2:21]Cl)[O:18][N:17]=3)[C:6]=2[CH:5]=[CH:4][CH:3]=1.[CH3:25][NH:26][CH3:27]>O1CCOCC1>[Cl:1][C:2]1[C:7]2[C:8](=[O:24])[N:9]([CH3:23])[CH2:10][C:11]3[N:12]([CH:13]=[N:14][C:15]=3[C:16]3[N:20]=[C:19]([CH2:21][N:26]([CH3:27])[CH3:25])[O:18][N:17]=3)[C:6]=2[CH:5]=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 674DimethylamineHCID 224621917-Chloro-3-(5-chloromethyl-[1,2,4]oxadiazol-3-yl)-5-methyl-4,5-dihydro-imidazo[1,5-a][1,4]benzodiazepin-6-one

생성물 1

HCID 9885841Evt-201

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

7.0 g 7-Chloro-3-(5-chloromethyl-[1,2,4]oxadiazol-3-yl)-5-methyl-4,5-dihydro-imidazo-[1,5-a][1,4]benzodiazepin-6-one were suspended under stirring and argon atmosphere in 70 ml 1,4-dioxane and 25.7 ml dimethylamine (33% in ethanol) were added over 60 minutes. The reaction mixture was stirred one more hour at r.t. and then the solvents were removed under reduced pressure at 35° C. The residue was partitioned between 50 ml dichloromethane and 20 ml deionized water. The phases were separated and the organic phase was washed twice with 20 ml deionized water. The aqueous phases were extracted separately with the same portion of 25 ml dichloromethane, twice. The combined organic extracts were dried (Na2SO4) and the solvent was removed under reduced pressure. Crude product: 8.0 g as a light yellow foam.

후처리

  1. stirringThe reaction mixture was stirred one more hour at r.t.
  2. customthe solvents were removed under reduced pressure at 35° C
  3. customThe residue was partitioned between 50 ml dichloromethane and 20 ml
  4. customThe phases were separated
  5. washthe organic phase was washed twice with 20 ml
  6. extractionThe aqueous phases were extracted separately with the same portion of 25 ml dichloromethane
  7. dry with materialThe combined organic extracts were dried (Na2SO4)
  8. customthe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-e170966746f54cfe9be2b0fdaa7f4716
출처 데이터셋
uspto-grants-2001_08
특허 번호
US06281353B1

반응 노트

불러오는 중…