Tris(hydroxymethyl)aminomethane → N-(1-((3,5-dimethylisoxazol-4-yl)methyl)-1H-pyrazol-4-yl)benzo[d][1,3]dioxole-5-carboxamide

HRID 548012

반응식

HRID 548012 반응식
Cl.[CH3:2][C:3]1[C:7]([CH2:8][N:9]2[CH:13]=[C:12]([NH2:14])[CH:11]=[N:10]2)=[C:6]([CH3:15])[O:5][N:4]=1.[O:16]1[C:20]2[CH:21]=[CH:22][C:23]([C:25](O)=[O:26])=[CH:24][C:19]=2[O:18][CH2:17]1.OC1C2N=NNC=2C=CC=1.C(O)C(N)(CO)CO>CN(C)C=O.C(#N)C>[CH3:2][C:3]1[C:7]([CH2:8][N:9]2[CH:13]=[C:12]([NH:14][C:25]([C:23]3[CH:22]=[CH:21][C:20]4[O:16][CH2:17][O:18][C:19]=4[CH:24]=3)=[O:26])[CH:11]=[N:10]2)=[C:6]([CH3:15])[O:5][N:4]=1

참가 물질

7

실험 절차

1-((3,5-dimethylisoxazol-4-yl)methyl)-1H-pyrazol-4-amine hydrochloride (example 1a) (8 mg, 35 μmol) and benzo[d][1,3]dioxole-5-carboxylic acid (7 mg, 42 μmol) were each dissolved in 200 uL dimethylformamide. Si-Carbodiimide resin (70 mg, 70 μmol) was loaded into a 1.2 mL 96 well Greiner plate, followed by the addition of amine and acid. Hydroxybenzotriazole (6 mg, 42 μmol) was dissolved in 100 uL dimethylformamide and was added into the reaction well. The reaction was shaken overnight at room temperature. To remove excess carboxylic acid and hydroxybenzotriazole, PS-Trisamine resin (35 mg, 70 μmol) was added into the reaction mixture and was allowed to shake overnight at room temperature. 200 uL of Acetonitrile was added into the reaction well and shaken for 1 minute. The top clear solution was transferred into a new plate. The extraction process was repeated two more times. The solution was evaporated under vacuum and gave the desired product.

후처리

  1. additionwas added into the reaction well
  2. additionwas added into the reaction mixture
  3. waitto shake overnight at room temperature
  4. stirringshaken for 1 minute
  5. customThe solution was evaporated under vacuum

출처 및 근거

ORD 기록
ord-fa1f933f40374b9985f64408d40ba93c
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07939671B2

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