4-[5-methyl-7-(3-nitro-phenyl)-benzo[1,2,4]triazin-3-yl amino]-N-(2-pyrrolidin-1-yl-ethyl)-benzenesulfonamide → HCID 44425267, 화합물

HRID 273528

반응식

HRID 273528 반응식
[CH3:1][C:2]1[C:7]2[N:8]=[C:9]([NH:12][C:13]3[CH:18]=[CH:17][C:16]([S:19]([NH:22][CH2:23][CH2:24][N:25]4[CH2:29][CH2:28][CH2:27][CH2:26]4)(=[O:21])=[O:20])=[CH:15][CH:14]=3)[N:10]=[N:11][C:6]=2[CH:5]=[C:4]([C:30]2[CH:35]=[CH:34][CH:33]=[C:32]([N+:36]([O-])=O)[CH:31]=2)[CH:3]=1>[Pd]>[NH2:36][C:32]1[CH:31]=[C:30]([C:4]2[CH:3]=[C:2]([CH3:1])[C:7]3[N:8]=[C:9]([NH:12][C:13]4[CH:14]=[CH:15][C:16]([S:19]([NH:22][CH2:23][CH2:24][N:25]5[CH2:26][CH2:27][CH2:28][CH2:29]5)(=[O:20])=[O:21])=[CH:17][CH:18]=4)[N:10]=[N:11][C:6]=3[CH:5]=2)[CH:35]=[CH:34][CH:33]=1

참가 물질

3

반응물 1

HCID 598376844-[5-methyl-7-(3-nitro-phenyl)-benzo[1,2,4]triazin-3-yl amino]-N-(2-pyrrolidin-1-yl-ethyl)-benzenesulfonamide

생성물 1

HCID 44425267HCID 44425267, 화합물수율 99.3%

시약·촉매·용매 1

HCID 23938Palladium촉매

실험 절차

4-[5-methyl-7-(3-nitro-phenyl)-benzo[1,2,4]triazin-3-yl amino]-N-(2-pyrrolidin-1-yl-ethyl)-benzenesulfonamide (0.16 g, 0.3 mmol, 1 equiv) was combined with 10% palladium on carbon (0.135 g) and flushed with argon. The reactants were then diluted with methanol (15 mL), and rthe eaction atmosphere was evacuated and replaced with hydrogen. A hydrogen balloon was affixed and the reaction was allowed to stir for 3 hours. Argon was then bubbled through the reaction mixture and the contents were filtered though a pad of Celite. The solvents were evaporated to provide the product as an orange solid (0.15 g, 98% yield). MS (ESI+): m/z=504.6, LC retention time: 1.84 min. 1H NMR (DMSO-d6): δ 1.64 (bs, 4H), 2.72 (s, 3H), 2.87 (bs, 2H), 5.26 (s, 2H), 6.65 (d, J=7.8 Hz, 1H), 7.00 (d, J=8.1 Hz, 1H), 7.05 (m, 1H), 7.18 (t, J=7.8 Hz, 1H), 7.83 (d, J=8.8 Hz, 2H), 8.12 (s, 1H), 8.21 (d, J=8.8 Hz, 2H), 8.27 (d, J=1.7 Hz, 1H), 11.44 (s, 1H).

후처리

  1. customflushed with argon
  2. additionThe reactants were then diluted with methanol (15 mL)
  3. customrthe eaction atmosphere was evacuated
  4. customArgon was then bubbled through the reaction mixture
  5. filtrationthe contents were filtered though a pad of Celite
  6. customThe solvents were evaporated

출처 및 근거

ORD 기록
ord-18a5e4757cbd4f35bd1e14e23b7b8760
출처 데이터셋
uspto-grants-2008_11
특허 번호
US07456176B2

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