4-(5-Nitro-2-trifluoromethoxy-phenyl)-piperazine-1-carboxylic acid tert-butyl ester → HCID 67095373、化合物

HRID 1710601

反応式

HRID 1710601 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:19]=[C:18]([N+:20]([O-])=O)[CH:17]=[CH:16][C:15]=2[O:23][C:24]([F:27])([F:26])[F:25])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]>C(OCC)(=O)C.C(O)(=O)C.[Pd]>[C:1]([O:5][C:6]([N:8]1[CH2:9][CH2:10][N:11]([C:14]2[CH:19]=[C:18]([NH2:20])[CH:17]=[CH:16][C:15]=2[O:23][C:24]([F:26])([F:27])[F:25])[CH2:12][CH2:13]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]

参加物

5

反応物 1

HCID 670947894-(5-Nitro-2-trifluoromethoxy-phenyl)-piperazine-1-carboxylic acid tert-butyl ester

生成物 1

HCID 67095373HCID 67095373、化合物収率 97.6%

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 176Acetic Acid溶媒HCID 8857Ethyl Acetate溶媒

実験手順

0.41 g of 4-(5-Nitro-2-trifluoromethoxy-phenyl)-piperazine-1-carboxylic acid tert-butyl ester (1.055 mmol) were dissolved in 10 mL ethyl acetate and 10 mL acetic acid. 0.12 g 10% Palladium/charcoal were added and the mixture hydrogenated for 3 h at room temperature. The catalyst was filtered over Celite, washed with ethyl acetate and the combined filtrates evaporated to dryness. The residue was treated with water, the pH adjusted to 9-10 with 1 N aquous sodium hydroxide and the aquous phase extracted twice with dichloromethane. The combined organic extracts were dried over magnesium sulfate, filtered, and the solvent evaporated under reduced pressure to yield 0.372 g of the product.

後処理

  1. filtrationThe catalyst was filtered over Celite
  2. washwashed with ethyl acetate
  3. customthe combined filtrates evaporated to dryness
  4. additionThe residue was treated with water
  5. extractionthe aquous phase extracted twice with dichloromethane
  6. dry with materialThe combined organic extracts were dried over magnesium sulfate
  7. filtrationfiltered
  8. customthe solvent evaporated under reduced pressure

出典と根拠

ORDレコード
ord-2bedcfa7abc741f2aa34ba263ce6204c
出典データセット
uspto-grants-2010_09
特許番号
US07790727B2

関連ノート

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