Hydrochloric Acid → N-(7-hydroxy-5,6-dihydro-7H-cyclopenta[d]pyrimidin-4-yl)-4-[3-(1-benzylpiperidin-4-yl)propanoyl]aniline

HRID 976136ノート

反応式

HRID 976136 の反応式
[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([CH2:14][CH2:15][C:16]([C:18]2[CH:24]=[CH:23][C:21]([NH2:22])=[CH:20][CH:19]=2)=[O:17])[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C([O:28][CH:29]1[C:33]2[N:34]=[CH:35][N:36]=[C:37](Cl)[C:32]=2[CH2:31][CH2:30]1)(=O)C.Cl.C[O-].[Na+].CO>C(O)C>[OH:28][CH:29]1[C:33]2[N:34]=[CH:35][N:36]=[C:37]([NH:22][C:21]3[CH:20]=[CH:19][C:18]([C:16](=[O:17])[CH2:15][CH2:14][CH:11]4[CH2:12][CH2:13][N:8]([CH2:1][C:2]5[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=5)[CH2:9][CH2:10]4)=[CH:24][CH:23]=3)[C:32]=2[CH2:31][CH2:30]1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 199689194-[3-(1-Benzylpiperidin-4-yl)propanoyl]anilineHCID 199689354-chloro-6,7-dihydro-5H-cyclopenta[d]pyrimidin-7-yl acetateHCID 23694274Sodium methanolate methanol

生成物 1

HCID 19968940N-(7-hydroxy-5,6-dihydro-7H-cyclopenta[d]pyrimidin-4-yl)-4-[3-(1-benzylpiperidin-4-yl)propanoyl]aniline収率 57.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

To 15 ml of ethanol were added 0.60 g of 4-[3-(1-benzylpiperidin-4-yl)propanoyl]aniline and 0.51 g of 7-acetoxy-4-chloro-5,6-dihydro-7H-cyclopenta[d]pyrimidine, then 3 ml of an ethanol solution of hydrochloric acid (containing 0.19 g of hydrochloric acid) was added to the mixture and the mixture was reacted under reflux for 30 minutes. After cooling, a 28% sodium methylate-methanol solution was added to the reaction mixture to make it alkaline, and the mixture was condensed under reduced pressure. The obtained residue was applied to silica gel column chromatography to obtain 0.49 g of the title compound as white crystal.

後処理

  1. customthe mixture was reacted
  2. temperatureunder reflux for 30 minutes
  3. temperatureAfter cooling
  4. customcondensed under reduced pressure

出典と根拠

ORDレコード
ord-28ec64a23db74abfbf55781afeece2a5
出典データセット
uspto-grants-1997_03
特許番号
US05610303

反応ノート

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