Hydrochloric Acid → Ethyl 7-hydroxychromane-2-carboxylate

HRID 479631

반응식

HRID 479631 반응식
[OH:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6](=O)[CH:7]=[C:8]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[O:9]2)=[CH:4][CH:3]=1.Cl>[Pd].CCO>[CH2:15]([O:14][C:12]([CH:8]1[CH2:7][CH2:6][C:5]2[C:10](=[CH:11][C:2]([OH:1])=[CH:3][CH:4]=2)[O:9]1)=[O:13])[CH3:16]

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 5376802ethyl 7-hydroxy-4-oxo-4H-chromen-2-carboxylate

생성물 1

HCID 11085381Ethyl 7-hydroxychromane-2-carboxylate

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

To a large hydrogenation vessel were added ethyl 7-hydroxychromone-2-carboxylate (=ethyl 7-hydroxy-4-oxo-4H-chromene-2-carboxylate) (675.4 g, 2.88 mol), EtOH 4 liters, conc. hydrochloric acid 40 ml. The resulting suspension was combined with 5% Pd/C 68 g, and subjected to hydrogenation condition (H2, 40 psi, rt) overnight. The reaction mixture was filtered through a pad of celite to remove the catalyst. The filtrate was concentrated to give thick oily material, which solidified upon standing. Tan solid 630.1 g (98%).

후처리

  1. customsubjected to hydrogenation condition (H2, 40 psi, rt) overnight
  2. filtrationThe reaction mixture was filtered through a pad of celite
  3. customto remove the catalyst
  4. concentrationThe filtrate was concentrated
  5. customto give thick oily material, which

출처 및 근거

ORD 기록
ord-45bd43d11af8419883022319c3127fb9
출처 데이터셋
uspto-grants-2003_11
특허 번호
US06645997B2

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