Dichloromethane → HCID 67975419、化合物

HRID 623882ノート

反応式

HRID 623882 の反応式
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]

参加物

6

反応物 4

HCID 6344DichloromethaneHCID 11430Potassium CarbonateHCID 67973239HCID 67973239、化合物HCID 866981711382999-80-5

生成物 1

HCID 67975419HCID 67975419、化合物収率 61%

試薬・触媒・溶媒 1

HCID 57417360Sodium chloride; water溶媒

反応条件

温度
50 °C

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-0eb09358f7a9409da5d2ac7470a64b4d
出典データセット
uspto-grants-2016_04
特許番号
US09302996B2

反応ノート

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