Hydrochloric Acid → 4-(5-Bromopyridin-3-yl)-2-(6-piperidin-1-ylpyrimidin-4-yl)-1,2-dihydro-3H-pyrazol-3-one hydrochloride

HRID 37904ノート

反応式

HRID 37904 の反応式
C[N:2](C)[CH:3]=[C:4]([C:10]1[CH:11]=[N:12][CH:13]=[C:14]([Br:16])[CH:15]=1)[C:5]([O:7]CC)=O.[NH:18]([C:20]1[CH:25]=[C:24]([N:26]2[CH2:31][CH2:30][CH2:29][CH2:28][CH2:27]2)[N:23]=[CH:22][N:21]=1)N.C1(C)C=CC(S(O)(=O)=O)=CC=1.[ClH:43]>C(O)C.O1CCOCC1>[ClH:43].[Br:16][C:14]1[CH:15]=[C:10]([C:4]2[C:5](=[O:7])[N:18]([C:20]3[CH:25]=[C:24]([N:26]4[CH2:27][CH2:28][CH2:29][CH2:30][CH2:31]4)[N:23]=[CH:22][N:21]=3)[NH:2][CH:3]=2)[CH:11]=[N:12][CH:13]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 6101p-Toluenesulfonic acidHCID 441403054-Hydrazinyl-6-(piperidin-1-yl)pyrimidineHCID 68799628Ethyl 3-(dimethylamino)-2-(5-bromopyridin-3-yl)acrylate

生成物 1

HCID 708727884-(5-Bromopyridin-3-yl)-2-(6-piperidin-1-ylpyrimidin-4-yl)-1,2-dihydro-3H-pyrazol-3-one hydrochloride

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 312751,4-Dioxane溶媒

実験手順

At 100° C., 500 mg (1.7 mmol) of the compound from Example 11A, 323 mg (1.7 mmol) of the compound from Example 8A and 58 mg (0.3 mmol) of p-toluenesulfonic acid are stirred in 2 ml of ethanol for 16 h. After cooling to RT, 0.5 ml of a 4 N solution of hydrogen chloride in dioxane is added, and the mixture is stirred at RT for 30 min. The precipitate is filtered off, washed first with ethanol and then with diethyl ether and dried under reduced pressure.

後処理

  1. filtrationThe precipitate is filtered off
  2. washwashed first with ethanol
  3. dry with materialwith diethyl ether and dried under reduced pressure

出典と根拠

ORDレコード
ord-40fc70cdf6ed40c89e12b09e7ec707d0
出典データセット
uspto-grants-2013_09
特許番号
US08524699B2

反応ノート

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