Formaldehyde → 1-Ethyl-4-(hydroxymethyl)piperazine-2,3-dione

HRID 1018447

반응식

HRID 1018447 반응식
[CH2:1]([N:3]1[CH2:8][CH2:7][NH:6][C:5](=[O:9])[C:4]1=[O:10])[CH3:2].[CH2:11]=[O:12]>Cl>[CH2:1]([N:3]1[CH2:8][CH2:7][N:6]([CH2:11][OH:12])[C:5](=[O:9])[C:4]1=[O:10])[CH3:2]

참가 물질

4

반응물 2

HCID 712FormaldehydeHCID 1088121-Ethyl-2,3-piperazinedione

생성물 1

HCID 184014561-Ethyl-4-(hydroxymethyl)piperazine-2,3-dione수율 100%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

반응 조건

온도
50 °C

실험 절차

To a solution of 1-ethylpiperazine-2,3-dione (2.13 g, 15 mmol) in 30% aqueous (methanol free) formaldehyde (15 mmol) potassium hydroxide (150 mg, 2.7 mmol) was added and the mixture stirred at 50° C. for 7 days. It was neutralized with 5 N aqueous hydrochloric acid (50 μl) to pH=7. The mixture was evaporated at 15 mm and then dried in high vacuo (0.0013 mbar) (0.001 mm) to give 1-ethyl-4- (hydroxymethyl)-piperazine-2,3-dione as a colourless solid (100%). NMR-spectrum in CDCl3: 1.15 (broad signal, 1H), 1.15 (t, 3H, J=7 Hz), 3.47 (q, 2H, J=7 Hz), 3.54 (m, 2H), 3.68 (m, 2H), 4.88 (s, 2H) ppm.

후처리

  1. customThe mixture was evaporated at 15 mm
  2. customdried in high vacuo (0.0013 mbar) (0.001 mm)

출처 및 근거

ORD 기록
ord-1896bacf1ee24ef1b74871aae3e5d2e0
출처 데이터셋
uspto-grants-2002_11
특허 번호
US06482818B2

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