Piperazine → 1-Boc-4-(2-piperazin-1-yl-benzoyl)-piperazine

HRID 1592709ノート

反応式

HRID 1592709 の反応式
[C:1]([N:8]1[CH2:13][CH2:12][N:11]([C:14](=[O:22])[C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2Br)[CH2:10][CH2:9]1)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].[NH:23]1[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]1>>[C:1]([N:8]1[CH2:13][CH2:12][N:11]([C:14](=[O:22])[C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[N:23]2[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]2)[CH2:10][CH2:9]1)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2]

参加物

3

反応物 2

HCID 4837PiperazineHCID 17952334Tert-butyl 4-(2-bromobenzoyl)piperazine-1-carboxylate

生成物 1

HCID 694101761-Boc-4-(2-piperazin-1-yl-benzoyl)-piperazine

実験手順

Boc protected piperazine (849 mg, 4.56 mmol) was dissolved in DCM (20 mL) and triethyl amine (2.54 mL, 18.2 mmol) was added. To the stirred solution, ortho-bromo benzoyl chloride (2 g, 9.11 mmol) was added via syringe under nitrogen. The system was stirred for about 12 hours at r.t. The reaction was washed with water, dried, filtered, and concentrated. The residue was subjected to chromatography on silica gel to give 1-Boc-4-(2-bromo-)-piperazine (1.48 g, 8.85 mmol) as a white foam. 1-Boc-4-(2-bromo-benzoyl)-piperazine was coupled to piperazine in a manner similar to Preparation 1A. LRMS (ESI+): 375.2 (M+1)

出典と根拠

ORDレコード
ord-9082b4a557f14a0db95363dc56e97111
出典データセット
uspto-grants-2007_11
特許番号
US07291619B2

反応ノート

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