4-Phenylpiperidinium chloride → HCID 18001212、化合物

HRID 478201ノート

反応式

HRID 478201 の反応式
Cl.[C:2]1([CH:8]2[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]2)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Cl:14][CH2:15][CH2:16][CH2:17][N:18]1[CH2:23][CH2:22][CH:21]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[CH2:20][CH2:19]1.ClCCCN1CCCC(C2C=CC(OC)=CC=2)C1>>[ClH:14].[C:2]1([CH:8]2[CH2:9][CH2:10][N:11]([CH2:15][CH2:16][CH2:17][N:18]3[CH2:19][CH2:20][CH:21]([C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=4)[CH2:22][CH2:23]3)[CH2:12][CH2:13]2)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 3

HCID 825094-Phenylpiperidinium chlorideHCID 2036891-(3-Chloropropyl)-4-phenylpiperidineHCID 18001200HCID 18001200、化合物

生成物 1

HCID 18001212HCID 18001212、化合物収率 66.4%

実験手順

Using 4-phenylpiperidine hydrochloride (99 mg, 0.50 mmol) ′and 1-(3-chloropropyl)-4-phenylpiperidine 2 hydrochloride (110 mg, 0.40 mmol) instead of 4-(3-indolyl)piperidine and 1-(3-chloropropyl)-3-(4-methoxyphenyl)piperidine 3 hydrochloride, respectively, the reaction and purification were carried out in the same procedure as Example 2. The resulting crude product was purified by column chromatography on a silica gel (silica gel NH-DM 1020 produced by Fuji Silysia Chemical Ltd., eluent; hexane:ether=2:1) to afford a free form (106 mg) of the title compound as white crystals. After adding hydrochloric acid/methanol to a solution of the free form in methanol, the mixture was concentrated and was then recrystallized from methanol/ether to afford the title compound (113 mg, yield: 65%) as white crystals.

後処理

  1. customrespectively, the reaction and purification
  2. customThe resulting crude product was purified by column chromatography on a silica gel (silica gel NH-DM 1020 produced by Fuji Silysia Chemical Ltd., eluent; hexane:ether=2:1)

出典と根拠

ORDレコード
ord-833293e0b13049e4a0bf79e0f1a43bfd
出典データセット
uspto-grants-2003_11
特許番号
US06642228B1

反応ノート

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