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

HRID 404642노트

반응식

HRID 404642 반응식
[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]

참가 물질

5

반응물 2

HCID 3939Lithium Hydroxide2회HCID 86688901Ethyl 2-(4-methyl-3-oxopiperazin-1-yl)-2-phenylacetate

생성물 1

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

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-da88808140474518a6dd0622ba16c240
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08748613B2

반응 노트

불러오는 중…