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Hydrochloric Acid → 1-Benzoyl-3-(3,4-dichlorophenyl)-3-[3-[4-(2-thenoylamino)-4-phenyl-piperid-1-yl]propyl]piperidine hydrochloride monohydrate

HRID 377815
ノート
印刷プレビュー

反応式

HRID 377815 の反応式
[NH2:1][C:2]1([C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)[CH2:7][CH2:6][N:5]([CH2:8][CH2:9][CH2:10][C:11]2([C:25]3[CH:30]=[CH:29][C:28]([Cl:31])=[C:27]([Cl:32])[CH:26]=3)[CH2:16][CH2:15][CH2:14][N:13]([C:17](=[O:24])[C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[CH2:12]2)[CH2:4][CH2:3]1.C(N(CC)CC)C.[C:46]1([C:51](Cl)=[O:52])[S:50][CH:49]=[CH:48][CH:47]=1.Cl>C(Cl)Cl>[OH2:24].[ClH:31].[C:17]([N:13]1[CH2:14][CH2:15][CH2:16][C:11]([C:25]2[CH:30]=[CH:29][C:28]([Cl:31])=[C:27]([Cl:32])[CH:26]=2)([CH2:10][CH2:9][CH2:8][N:5]2[CH2:4][CH2:3][C:2]([NH:1][C:51](=[O:52])[C:46]3[S:50][CH:49]=[CH:48][CH:47]=3)([C:33]3[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=3)[CH2:7][CH2:6]2)[CH2:12]1)(=[O:24])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 789282-Thiophenecarbonyl chlorideHCID 152855913-[3-(4-Amino-4-phenylpiperid-1-yl)propyl]-1-benzoyl-3-(3,4-dichlorophenyl)-piperidine

生成物 1

HCID 227417571-Benzoyl-3-(3,4-dichlorophenyl)-3-[3-[4-(2-thenoylamino)-4-phenyl-piperid-1-yl]propyl]piperidine hydrochloride monohydrate収率 101.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

This compound is prepared by the procedure described in step B of EXAMPLE 19, starting from 1.5 g of the compound obtained in step A of EXAMPLE 19, 0.55 g of triethylamine and 0.4 g of 2-thenoyl chloride in 10 ml of DCM. The residue is chromatographed on silica H using DCM and then a DCM/MeOH mixture (95/5; v/v) as the eluent. The product obtained is taken up with DCM and acidified to pH 1 by the addition of ethereal hydrogen chloride and the precipitate obtained is filtered off to give 0.99 g of the expected product, m.p.=198-200° C.

後処理

  1. customThis compound is prepared by the procedure
  2. customThe residue is chromatographed on silica H
  3. customThe product obtained
  4. customthe precipitate obtained
  5. filtrationis filtered off

出典と根拠

ORDレコード
ord-669982032ec44a87aeedbcbfb5197200
出典データセット
uspto-grants-2000_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06028082

反応ノート

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