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Potassium Carbonate → HCID 68525583、化合物

HRID 1932527
ノート
印刷プレビュー

反応式

HRID 1932527 の反応式
Cl.Cl.[Cl:3][C:4]1[CH:5]=[C:6]([CH:33]=[CH:34][C:35]=1[Cl:36])[C:7]([NH:9][C:10]1[CH:11]=[N:12][C:13]([O:16][C:17]2[CH:22]=[CH:21][C:20]([C:23]([N:25]3[CH2:30][CH2:29][CH:28]([NH:31][CH3:32])[CH2:27][CH2:26]3)=[O:24])=[CH:19][CH:18]=2)=[CH:14][CH:15]=1)=[O:8].Br[CH2:38][C:39]1[CH:44]=[CH:43][C:42]([F:45])=[C:41]([F:46])[CH:40]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[Cl:3][C:4]1[CH:5]=[C:6]([CH:33]=[CH:34][C:35]=1[Cl:36])[C:7]([NH:9][C:10]1[CH:11]=[N:12][C:13]([O:16][C:17]2[CH:18]=[CH:19][C:20]([C:23]([N:25]3[CH2:30][CH2:29][CH:28]([NH:31][CH2:32][CH2:38][C:39]4[CH:44]=[CH:43][C:42]([F:45])=[C:41]([F:46])[CH:40]=4)[CH2:27][CH2:26]3)=[O:24])=[CH:21][CH:22]=2)=[CH:14][CH:15]=1)=[O:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 5814364-(Bromomethyl)-1,2-difluorobenzeneHCID 68522239HCID 68522239、化合物

生成物 1

HCID 68525583HCID 68525583、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

3,4-dichloro-N-{6-[4-(4-methylamino-piperidine-1-carbonyl)phenoxy]pyridin-3-yl}benzamide dihydrochloride (114 mg, 0.2 mmol) was dissolved in DMF (3 mL). To the resulting solution were added 4-bromomethyl-1,2-difluorobenzene (31 μl, 0.24 mmol) and potassium carbonate (111 mg, 0.8 mmol), and this solution was stirred for 4 hours at room temperature. The resulting reaction solution was concentrated under reduced pressure. The residue was diluted with ethyl acetate and washed with water and brine. The organic layer was dried over anhydrous magnesium sulfate, and evaporated. This residue was purified by silica gel column chromatography (chloroform:methanol=50:1), to thereby yield 60 mg of the title compound.

後処理

  1. customThe resulting reaction solution
  2. concentrationwas concentrated under reduced pressure
  3. additionThe residue was diluted with ethyl acetate
  4. washwashed with water and brine
  5. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  6. customevaporated
  7. customThis residue was purified by silica gel column chromatography (chloroform:methanol=50:1)

出典と根拠

ORDレコード
ord-1ffaad16b7d74763990db02e544d2b24
出典データセット
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08188277B2

反応ノート

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