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

HRID 901331ノート

反応式

HRID 901331 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-5e7deb17ac814ff1907339b9a7fbd611
出典データセット
uspto-grants-2008_04
特許番号
US07361663B2

反応ノート

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