1,4'-Bipiperidine → 3-Methyl-2-[4-[6-(4-piperidinopiperidinyl)nicotinoyl]benzylthio]thieno[3,2-d]pyrimidin-4(3H)-one hydrochloride

HRID 1291348ノート

反応式

HRID 1291348 の反応式
[Cl:1][C:2]1[CH:28]=[CH:27][C:5]([C:6]([C:8]2[CH:26]=[CH:25][C:11]([CH2:12][S:13][C:14]3[N:15]([CH3:24])[C:16](=[O:23])[C:17]4[S:22][CH:21]=[CH:20][C:18]=4[N:19]=3)=[CH:10][CH:9]=2)=[O:7])=[CH:4][N:3]=1.[N:29]1([CH:35]2[CH2:40][CH2:39][NH:38][CH2:37][CH2:36]2)[CH2:34][CH2:33][CH2:32][CH2:31][CH2:30]1>N1C=CC=CC=1>[ClH:1].[CH3:24][N:15]1[C:16](=[O:23])[C:17]2[S:22][CH:21]=[CH:20][C:18]=2[N:19]=[C:14]1[S:13][CH2:12][C:11]1[CH:25]=[CH:26][C:8]([C:6](=[O:7])[C:5]2[CH:27]=[CH:28][C:2]([N:38]3[CH2:39][CH2:40][CH:35]([N:29]4[CH2:34][CH2:33][CH2:32][CH2:31][CH2:30]4)[CH2:36][CH2:37]3)=[N:3][CH:4]=2)=[CH:9][CH:10]=1

参加物

4

反応物 2

HCID 786071,4'-BipiperidineHCID 189187982-[4-(6-Chloronicotinoyl)benzylthio]-3-methylthieno[3,2-d]pyrimidin-4(3H)-one

生成物 1

HCID 189192833-Methyl-2-[4-[6-(4-piperidinopiperidinyl)nicotinoyl]benzylthio]thieno[3,2-d]pyrimidin-4(3H)-one hydrochloride収率 62.7%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A solution of 2-[4-(6-chloronicotinoyl]benzylthio]-3-methylthieno[3,2-d]pyrimidin-4(3H)-one (427 mg) and 4-piperidinopiperidine (202 mg) in pyridine (10 ml) was stirred at 80° C. for 10 hours. This reaction mixture was concentrated, the residue was dissolved in chloroform, and the solution was washed with water, dried, and concentrated. The residue was purified by silica gel column chromatography (chloroform: methanol: aqueous ammonia=50:1:0.1) and treated with HCl/ethyl acetate for conversion to hydrochloride to provide the title compound as colorless solid (373 mg).

後処理

  1. concentrationThis reaction mixture was concentrated
  2. dissolutionthe residue was dissolved in chloroform
  3. washthe solution was washed with water
  4. customdried
  5. concentrationconcentrated
  6. customThe residue was purified by silica gel column chromatography (chloroform: methanol: aqueous ammonia=50:1:0.1)
  7. additiontreated with HCl/ethyl acetate for conversion to hydrochloride

出典と根拠

ORDレコード
ord-abe6b376ec6e42ebb6d54766e2f5a4c8
出典データセット
uspto-grants-1998_05
特許番号
US05753664

反応ノート

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