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Hydrochloric Acid → HCID 58841411、化合物

HRID 32110
ノート
印刷プレビュー

反応式

HRID 32110 の反応式
[CH3:1][N:2]([CH3:18])[CH2:3][CH2:4][O:5][C:6]1[CH:7]=[C:8]2[C:13](=[CH:14][CH:15]=1)[C:12](=[N:16]O)[CH2:11][CH2:10][CH2:9]2.Cl>[Pd].CCO>[CH3:1][N:2]([CH3:18])[CH2:3][CH2:4][O:5][C:6]1[CH:7]=[C:8]2[C:13](=[CH:14][CH:15]=1)[CH:12]([NH2:16])[CH2:11][CH2:10][CH2:9]2
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 724406286-(2-dimethylamino-ethoxy)-3,4-dihydro-2H-naphthalen-1-one Oxime

生成物 1

HCID 58841411HCID 58841411、化合物

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

A mixture of 6-(2-dimethylamino-ethoxy)-3,4-dihydro-2H-naphthalen-1-one oxime (0.3 g, 1.2 mmol), EtOH (12 mL), Pd/C (Aldrich, 0.13g, 0.12 mmol), and concentrated HCl (0.24 mL) was purged with H2 and connected to a H2 balloon overnight at RT. The catalyst was filtered through Celite® and washed with MeOH. The filtrate was concentrated in vacuo. The residue was added saturated NaHCO3 and extracted with CH2Cl2. The organic solution was dried over Na2SO4, filtered and concentrated in vacuo. The crude product was purified by silica gel chromatography (5%-10% MeOH—CH2Cl2) to afford the compound as a colorless oil. MS (ESI): 235 (M+H)+.

後処理

  1. customwas purged with H2
  2. customconnected to a H2 balloon overnight at RT
  3. filtrationThe catalyst was filtered through Celite®
  4. washwashed with MeOH
  5. concentrationThe filtrate was concentrated in vacuo
  6. additionThe residue was added saturated NaHCO3
  7. extractionextracted with CH2Cl2
  8. dry with materialThe organic solution was dried over Na2SO4
  9. filtrationfiltered
  10. concentrationconcentrated in vacuo
  11. customThe crude product was purified by silica gel chromatography (5%-10% MeOH—CH2Cl2)

出典と根拠

ORDレコード
ord-6da1dde5e22f4bc7ada87f20850fec67
出典データセット
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07425631B2

反応ノート

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