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HCID 658603、化合物 → HCID 59570176、化合物

HRID 2070989
ノート
印刷プレビュー

反応式

HRID 2070989 の反応式
[C:1]([C:5]1[C:6]([OH:14])=[C:7]([CH:11]=[CH:12][CH:13]=1)[CH:8]=[N:9]O)([CH3:4])([CH3:3])[CH3:2]>CCOC(C)=O.CO.[Pd]>[NH2:9][CH2:8][C:7]1[CH:11]=[CH:12][CH:13]=[C:5]([C:1]([CH3:3])([CH3:2])[CH3:4])[C:6]=1[OH:14]
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 1

HCID 658603HCID 658603、化合物

生成物 1

HCID 59570176HCID 59570176、化合物収率 23.7%

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 887Methanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

3-tert-butyl-2-hydroxybenzaldehyde oxime (550 mg, 2.9 mmol) in EtOAc (10 mL) and MeOH (10 mL) was hydrogenated at balloon pressure in the presence of 10% Pd on carbon (100 mg) for 15 h. The reaction mixture was filtered over celite and concentrated. The residue was dissolved in EtOAc and 0.5 N HCl (10 mL). The layers were separated and the aqueous layer was treated with 1N NaOH solution until pH=9. The resulting aqueous layer was extracted with CHCl3 (3×10 mL). The combined CHCl3 was washed with brine, dried with Na2SO4 and concentrated under reduced pressure to provide to desired product (123 mg, 23%).

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. filtrationThe reaction mixture was filtered over celite and
  2. concentrationconcentrated
  3. dissolutionThe residue was dissolved in EtOAc
  4. customThe layers were separated
  5. additionthe aqueous layer was treated with 1N NaOH solution until pH=9
  6. extractionThe resulting aqueous layer was extracted with CHCl3 (3×10 mL)
  7. washThe combined CHCl3 was washed with brine
  8. dry with materialdried with Na2SO4
  9. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-5de46f2656064f058ede2a6f43fd8643
出典データセット
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08299267B2

反応ノート

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