Diisopropylethylamine → Ethyl 2-(4-methyl-3-oxopiperazin-1-yl)-2-phenylacetate

HRID 404641ノート

反応式

HRID 404641 の反応式
CCN(C(C)C)C(C)C.Cl.[CH3:11][N:12]1[CH2:17][CH2:16][NH:15][CH2:14][C:13]1=[O:18].Br[CH:20]([C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)[C:21]([O:23][CH2:24][CH3:25])=[O:22]>C(#N)C>[CH3:11][N:12]1[CH2:17][CH2:16][N:15]([CH:20]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[C:21]([O:23][CH2:24][CH3:25])=[O:22])[CH2:14][C:13]1=[O:18]

参加物

5

反応物 3

HCID 81531Diisopropylethylamine2 回HCID 97780Ethyl bromophenylacetateHCID 170607661-Methylpiperazin-2-one--hydrogen chloride (1/1)

生成物 1

HCID 86688901Ethyl 2-(4-methyl-3-oxopiperazin-1-yl)-2-phenylacetate収率 75.3%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

DIPEA (0.52 ml, 2.96 mmol) and 1-methylpiperazin-2-one hydrochloride (0.22 g, 1.48 mmol) were sequentially added to a solution of ethyl 2-bromo-2-phenylacetate (0.22 ml, 1.23 mmol) in acetonitrile (4 ml). The reaction was stirred at room temperature for 1.5 hours. DIPEA (0.13 ml, 0.74 mmol) was added again and the reaction was stirred at room temperature overnight. The solvent was evaporated and the crude was purified by flash chromatography (DCM/Acetone=9/1) to obtain ethyl 2-(4-methyl-3-oxopiperazin-1-yl)-2-phenylacetate (256 mg, 75% yield) as a yellow oil.

後処理

  1. stirringthe reaction was stirred at room temperature overnight
  2. customThe solvent was evaporated
  3. customthe crude was purified by flash chromatography (DCM/Acetone=9/1)

出典と根拠

ORDレコード
ord-f849d05d494e406c90618584cd5db001
出典データセット
uspto-grants-2014_06
特許番号
US08748613B2

反応ノート

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