HCID 69034741, 화합물 → Methyl 2-amino-4-[(tert-butoxycarbonyl)amino]benzoate

HRID 2215864노트

반응식

HRID 2215864 반응식
[CH3:1][O:2][C:3](=[O:21])[C:4]1[CH:9]=[CH:8][C:7]([NH:10][C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])=[CH:6][C:5]=1[N+:18]([O-])=O>C(OCC)(=O)C.[Pd]>[CH3:1][O:2][C:3](=[O:21])[C:4]1[CH:9]=[CH:8][C:7]([NH:10][C:11]([O:13][C:14]([CH3:15])([CH3:17])[CH3:16])=[O:12])=[CH:6][C:5]=1[NH2:18]

참가 물질

4

반응물 1

HCID 69034741HCID 69034741, 화합물

생성물 1

HCID 21056495Methyl 2-amino-4-[(tert-butoxycarbonyl)amino]benzoate수율 100.2%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 4-(tert-butoxycarbonylamino)-2-nitro-benzoic acid methyl ester (7.0 g, 23.6 mmoles) in 400 mL ethyl acetate was added 1.0 g 10% Pd/C. The reaction mixture was subjected to hydrogenation using a balloon for 24–36 hrs or until the reaction was complete as monitored by HPLC. The mixture was filtered through a celite bed, and the solid cake was thoroughly washed by ethyl acetate. The filtrate was concentrated in vacuo to dryness to afford the title compound (6.3 g, 99%). ES+ MS showed 267 m/z, the correct mass for the product.

후처리

  1. customfor 24–36 hrs
  2. filtrationThe mixture was filtered through a celite bed
  3. washthe solid cake was thoroughly washed by ethyl acetate
  4. concentrationThe filtrate was concentrated in vacuo to dryness

출처 및 근거

ORD 기록
ord-f0a9c4e1cd384922952fe2a7b0854bf4
출처 데이터셋
uspto-grants-2006_09
특허 번호
US07109332B2

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