2-tert-Butyl-7-nitro-6-phenyl-1,3-benzoxazole-4-carboxylic Acid → HCID 68584986、化合物

HRID 17517ノート

反応式

HRID 17517 の反応式
[C:1]([C:5]1[O:6][C:7]2[C:8](=[C:10]([C:23]([OH:25])=[O:24])[CH:11]=[C:12]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)[C:13]=2[N+:14]([O-])=O)[N:9]=1)([CH3:4])([CH3:3])[CH3:2].[H][H]>CO.[C].[Pd]>[NH2:14][C:13]1[C:12]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=[CH:11][C:10]([C:23]([OH:25])=[O:24])=[C:8]2[C:7]=1[O:6][C:5]([C:1]([CH3:4])([CH3:2])[CH3:3])=[N:9]2

参加物

5

反応物 2

HCID 685849732-tert-Butyl-7-nitro-6-phenyl-1,3-benzoxazole-4-carboxylic AcidHCID 178418361HCID 178418361、化合物

生成物 1

HCID 68584986HCID 68584986、化合物

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 887Methanol溶媒

実験手順

2-tert-Butyl-7-nitro-6-phenyl-1,3-benzoxazole-4-carboxylic acid (I-223) (6.27 mmol) was dissolved in methanol (30 ml), then at room temperature, 10% palladium-carbon (430 mg) was added. The suspension was stirred at room temperature under atmospheric pressure of hydrogen for 16 hour. The catalyst was removed by filtration with washing with methanol, and the filtrate was concentrated under reduced pressure. The resulting residue was purified by middle-pressure liquid chromatography (eluent, chloroform:methanol=98:2) to obtain the entitled compound (1.274 g, 66% from I-222) as a pale brown powder.

後処理

  1. customThe catalyst was removed by filtration
  2. washwith washing with methanol
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. customThe resulting residue was purified by middle-pressure liquid chromatography (eluent, chloroform:methanol=98:2)
  5. customto obtain the entitled compound (1.274 g, 66% from I-222) as a pale brown powder

出典と根拠

ORDレコード
ord-c0e17637b46140c89d172dc850b67008
出典データセット
uspto-grants-2010_06
特許番号
US07737166B2

反応ノート

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