Dichloromethane → HCID 67975419, 화합물

HRID 623882노트

반응식

HRID 623882 반응식
C(Cl)Cl.[C:4]([C:7]1[C:8]([CH3:28])=[CH:9][C:10]([C:13]2[CH:27]=[CH:26][C:16]([O:17][CH2:18][C:19]([CH3:25])([CH3:24])[C:20]([O:22][CH3:23])=[O:21])=[CH:15][CH:14]=2)=[N:11][CH:12]=1)(=[NH:6])[NH2:5].C(=O)([O-])[O-].[K+].[K+].Br[CH2:36][C:37]([C:39]1([C:42]([F:45])([F:44])[F:43])[CH2:41][CH2:40]1)=O>[Cl-].[Na+].O>[CH3:24][C:19]([CH3:25])([CH2:18][O:17][C:16]1[CH:26]=[CH:27][C:13]([C:10]2[CH:9]=[C:8]([CH3:28])[C:7]([C:4]3[NH:5][C:37]([C:39]4([C:42]([F:45])([F:44])[F:43])[CH2:41][CH2:40]4)=[CH:36][N:6]=3)=[CH:12][N:11]=2)=[CH:14][CH:15]=1)[C:20]([O:22][CH3:23])=[O:21]

참가 물질

6

반응물 4

HCID 6344DichloromethaneHCID 11430Potassium CarbonateHCID 67973239HCID 67973239, 화합물HCID 866981711382999-80-5

생성물 1

HCID 67975419HCID 67975419, 화합물수율 61%

시약·촉매·용매 1

HCID 57417360Sodium chloride; water용매

반응 조건

온도
50 °C

실험 절차

To methylene chloride (10 mL) and saturated brine (10 mL) were added methyl 3-[4-(5-carbamimidoyl-4-methylpyridin-2-yl)phenoxy]-2,2-dimethylpropanoate (500 mg) and potassium carbonate (430.3 mg), then, 2-bromo-1-[1-(trifluoromethyl)cyclopropyl]-ethanone (431.6 mg) was added to the mixture, and the resulting mixture was stirred at 50° C. overnight. The organic layer was separated and the residue obtained by concentrating the same under reduced pressure was purified by silica gel column chromatography (n-hexane:ethyl acetate=75:25 to 25:75) to obtain methyl 2,2-dimethyl-3-[4-(4-methyl-5-{5-[1-(trifluoromethyl)cyclopropyl]-1H-imidazol-2-yl}pyridin-2-yl)phenoxy]propanoate (423 mg).

후처리

  1. customThe organic layer was separated
  2. customthe residue obtained
  3. concentrationby concentrating the same under reduced pressure
  4. customwas purified by silica gel column chromatography (n-hexane:ethyl acetate=75:25 to 25:75)

출처 및 근거

ORD 기록
ord-0eb09358f7a9409da5d2ac7470a64b4d
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09302996B2

반응 노트

불러오는 중…