Triethylamine → 2,2-Dimethyl-5-(pyrrolidin-2-ylidene)-1,3-dioxane-4,6-dione

HRID 901331

반응식

HRID 901331 반응식
CO[C:3]1[CH2:4][CH2:5][CH2:6][N:7]=1.[C:8]1(=[O:17])[O:16][C:13]([CH3:15])([CH3:14])[O:12][C:10](=[O:11])[CH2:9]1.C(N(CC)CC)C>C1C=CC=CC=1>[CH3:14][C:13]1([CH3:15])[O:16][C:8](=[O:17])[C:9](=[C:3]2[CH2:4][CH2:5][CH2:6][NH:7]2)[C:10](=[O:11])[O:12]1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 162492,2-Dimethyl-1,3-dioxane-4,6-dioneHCID 3534432-Methoxy-1-Pyrroline

생성물 1

HCID 7085372,2-Dimethyl-5-(pyrrolidin-2-ylidene)-1,3-dioxane-4,6-dione수율 71.3%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

A solution of 5-Methoxy-3,4-dihydro-2H-pyrrole (5.35 g, 54.0 mmol), isopropylidene malonate (7.78 g, 54.0 mmol), triethylamine (1.35 mL, 9.7 mmol) and benzene (55 mL) is refluxed under nitrogen overnight. The reaction is cooled to RT and concentrated and the crude product is recrystalized from EtOH (95 mL) to give the title compound as a white solid (8.13 g, 38.5 mmol). 1H NMR (CDCl3, 300 MHz) 3.73(t, 2H), 3.35(t, 2H), 2.20-2.08(m, 2H), 1.66(s, 6H).

후처리

  1. concentrationconcentrated
  2. customthe crude product is recrystalized from EtOH (95 mL)

출처 및 근거

ORD 기록
ord-5e7deb17ac814ff1907339b9a7fbd611
출처 데이터셋
uspto-grants-2008_04
특허 번호
US07361663B2

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