4-Amino-2-methoxy-3-[(1-methyl-4-nitro-1H-pyrrole-2-carbonyl)-amino]-benzoic Acid Methyl Ester → HCID 178497318, 화합물

HRID 39663노트

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HRID 39663 반응식
[CH3:1][O:2][C:3](=[O:25])[C:4]1[CH:9]=[CH:8][C:7]([NH2:10])=[C:6]([NH:11][C:12]([C:14]2[N:15]([CH3:22])[CH:16]=[C:17]([N+:19]([O-:21])=[O:20])[CH:18]=2)=O)[C:5]=1[O:23][CH3:24]>C(O)(=O)C>[CH3:1][O:2][C:3]([C:4]1[CH:9]=[CH:8][C:7]2[N:10]=[C:12]([C:14]3[N:15]([CH3:22])[CH:16]=[C:17]([N+:19]([O-:21])=[O:20])[CH:18]=3)[NH:11][C:6]=2[C:5]=1[O:23][CH3:24])=[O:25]

참가 물질

3

반응물 1

HCID 120975624-Amino-2-methoxy-3-[(1-methyl-4-nitro-1H-pyrrole-2-carbonyl)-amino]-benzoic Acid Methyl Ester

생성물 1

HCID 178497318HCID 178497318, 화합물수율 85.5%

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
90 °C

실험 절차

The aforementioned mixture of amides 14a/14b (500 mg, 1.43 mmol) was suspended in glacial acetic acid (8 mL) and heated to 90° C. for 7 h. Most of the solvent was evaporated, and the yellow residue was suspended in Et2O. After being vigorously stirred for 20 min, the precipitate was filtered and washed with Et2O. Drying under hv gave 404 mg (85%) of 15 as a beige solid. Data of 15: Rf 0.80 (hexane/EtOAc 1:5). 1H NMR (300 MHz, DMSOd6): δ 3.76 (s, 3H), 4.14 (s, 3H), 4.34 (s, 3H), 7.14-7.17 (m, 1H), 7.48-7.55 (m, 3H), 8.25 (s, 1H). MS (ESI): m/z (rel intensity) 331 (98).

후처리

  1. customMost of the solvent was evaporated
  2. filtrationthe precipitate was filtered
  3. washwashed with Et2O
  4. customDrying under hv

출처 및 근거

ORD 기록
ord-470fd18e4c004da9bf043eb5c0be01eb
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08524899B2

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