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

HRID 17517노트

반응식

HRID 17517 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

HCID 68584986HCID 68584986, 화합물

시약·촉매·용매 2

HCID 178418390HCID 178418390, 화합물촉매HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c0e17637b46140c89d172dc850b67008
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07737166B2

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