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tert-Butyl piperazine-1-carboxylate → tert-Butyl 4-(2-(3,3-bis(4-chlorophenyl)-2-oxopyrrolidin-1-yl)acetyl)piperazine-1-carboxylate

HRID 2408854
ノート
印刷プレビュー

反応式

HRID 2408854 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2([C:18]3[CH:23]=[CH:22][C:21]([Cl:24])=[CH:20][CH:19]=3)[CH2:12][CH2:11][N:10]([CH2:13][C:14](O)=[O:15])[C:9]2=[O:17])=[CH:4][CH:3]=1.[N:25]1([C:31]([O:33][C:34]([CH3:37])([CH3:36])[CH3:35])=[O:32])[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]1.Cl.CN(C)CCCN=C=NCC>C(Cl)Cl.CN(C)C1C=CN=CC=1>[Cl:24][C:21]1[CH:22]=[CH:23][C:18]([C:8]2([C:5]3[CH:4]=[CH:3][C:2]([Cl:1])=[CH:7][CH:6]=3)[CH2:12][CH2:11][N:10]([CH2:13][C:14]([N:28]3[CH2:27][CH2:26][N:25]([C:31]([O:33][C:34]([CH3:37])([CH3:36])[CH3:35])=[O:32])[CH2:30][CH2:29]3)=[O:15])[C:9]2=[O:17])=[CH:19][CH:20]=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 3

HCID 143452tert-Butyl piperazine-1-carboxylateHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 673873472-(3,3-Bis(4-chlorophenyl)-2-oxopyrrolidin-1-yl)acetic acid

生成物 1

HCID 86657628tert-Butyl 4-(2-(3,3-bis(4-chlorophenyl)-2-oxopyrrolidin-1-yl)acetyl)piperazine-1-carboxylate

試薬・触媒・溶媒 2

HCID 14284
4-(Dimethylamino)pyridine
触媒
HCID 6344Dichloromethane溶媒

実験手順

To a solution of the product from Example 25D (0.8 g, 2.2 mmol) in CH2Cl2 (30 mL) was added tert-butyl piperazine-1-carboxylate (0.41 g, 2.2 mmol) under nitrogen. 1-(3-Dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (0.84 g, 4.4 mmol) and 4-(dimethylamino)pyridine (0.027 g, 0.22 mmol) were added, and the reaction mixture was stirred overnight at room temperature. The reaction mixture was then washed with water and brine, dried over MgSO4, filtered, and concentrated. The crude product was purified by chromatography on silica gel (Analogix Intelliflash 280; (CH3OH/CH2Cl2, 2:98 eluant) to afford the title compound.

後処理

  1. washThe reaction mixture was then washed with water and brine
  2. dry with materialdried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe crude product was purified by chromatography on silica gel (Analogix Intelliflash 280

出典と根拠

ORDレコード
ord-aa43a0dc2ae9417f8d79906d9e984c55
出典データセット
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08815869B2

反応ノート

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