Lithium Hydroxide → 2-(4-Methyl-3-oxopiperazin-1-yl)-2-phenylacetic acid

HRID 404642ノート

反応式

HRID 404642 の反応式
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([CH:8]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[C:9]([O:11]CC)=[O:10])[CH2:4][C:3]1=[O:20].[OH-].[Li+]>C(O)C.O>[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([CH:8]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[C:9]([OH:11])=[O:10])[CH2:4][C:3]1=[O:20]

参加物

5

反応物 2

HCID 3939Lithium Hydroxide2 回HCID 86688901Ethyl 2-(4-methyl-3-oxopiperazin-1-yl)-2-phenylacetate

生成物 1

HCID 584907532-(4-Methyl-3-oxopiperazin-1-yl)-2-phenylacetic acid収率 76.1%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

Ethyl 2-(4-methyl-3-oxopiperazin-1-yl)-2-phenylacetate (250 mg, 0.90 mmol) was dissolved in ethanol (8.6 ml) and water (4.3 ml). Lithium hydroxide (28.2 mg, 1.18 mmol) was added and the reaction was stirred at room temperature for three days. A second portion of lithium hydroxide (4.33 mg, 0.18 mmol) was added and the reaction was stirred at room temperature for 24 hours. EtOH was evaporated and 1N HCl was added to the aqueous solution till pH 7. The water was evaporated and the residue was suspended in acetonitrile and filtered on a buckner funnel washing with acetonitrile to obtain 170 mg of desired compound as a white solid. The compound was used in the next step without any further purification.

後処理

  1. stirringthe reaction was stirred at room temperature for 24 hours
  2. customEtOH was evaporated
  3. addition1N HCl was added to the aqueous solution till pH 7
  4. customThe water was evaporated
  5. filtrationfiltered on a buckner funnel
  6. washwashing with acetonitrile

出典と根拠

ORDレコード
ord-da88808140474518a6dd0622ba16c240
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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