Hydrochloric Acid → HCID 66675741、化合物

HRID 2377094

反応式

HRID 2377094 の反応式
[CH2:1]1[C:9]2[CH:8]=[CH:7][N:6]=[CH:5][C:4]=2[C:3](=[O:10])[NH:2]1.Cl.O1CCOCC1>O=[Pt]=O.CC(O)=O>[CH2:1]1[CH:9]2[CH:4]([CH2:5][NH:6][CH2:7][CH2:8]2)[C:3](=[O:10])[NH:2]1

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 205051661,2-Dihydro-3H-pyrrolo(3,4-c)pyridin-3-one

生成物 1

HCID 66675741HCID 66675741、化合物収率 138.3%

試薬・触媒・溶媒 2

HCID 345198Adams' catalyst触媒HCID 176Acetic Acid溶媒

実験手順

1,2-dihydro-3H-pyrrolo[3,4-c]pyridine-3-one (19.6 g, 0.146 mol) was placed into a hydrogenation reactor together with 250 mL AcOH and 1 g of PtO2 (Colonial Metals). An H2 pressure of 60 PSI was applied and the mixture hydrogenated until a pressure of 26 PSI was measured. The reaction mixture was filtered and the solvent evaporated. At the end of the evaporation, 4 N HCl in 1,4-dioxane (50 mL, 0.2 mol) was added. The solvent was evaporated to dryness. Ether (800 mL) was added and the mixture was stirred and filtered. The filter, a white solid, was dried to give 28.3 g of the desired product. 1H NMR (300 MHz, d6-DMSO) δ=9.42 (br s, 1H), 8.33 (br s, 1H), 7.88 (s, 1H), 3.44-3.25 (m, overlaps with water peak, observed integral of 6H includes water), 3.11-3.01 (m, 2H), 2.88-2.76 (m, 2H), 2.64 (br t, 1H), 2.55-2.45 (m, 3H) 1.90-1.75 (m, 1H), 1.61-1.42 (m, 1H). LCMS: 1.0 min, M+H=144.1 u/e.

後処理

  1. filtrationThe reaction mixture was filtered
  2. customthe solvent evaporated
  3. additionwas added
  4. customThe solvent was evaporated to dryness
  5. additionEther (800 mL) was added
  6. filtrationfiltered
  7. customThe filter, a white solid, was dried

出典と根拠

ORDレコード
ord-254d064c0ab44d64b0d0d69eecedf2e6
出典データセット
uspto-grants-2008_12
特許番号
US07468375B2

関連ノート

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