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

HRID 548012
ノート
印刷プレビュー

反応式

HRID 548012 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 6503Tris(hydroxymethyl)aminomethaneHCID 71961,3-Benzodioxole-5-carboxylic acidHCID 574222641-((3,5-dimethylisoxazol-4-yl)methyl)-1H-pyrazol-4-amine hydrochlorideHCID 178418300HCID 178418300、化合物2 回

生成物 1

HCID 57422267N-(1-((3,5-dimethylisoxazol-4-yl)methyl)-1H-pyrazol-4-yl)benzo[d][1,3]dioxole-5-carboxamide収率 6%

試薬・触媒・溶媒

2
HCID 6228Dimethylformamide溶媒2 回HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-fa1f933f40374b9985f64408d40ba93c
出典データセット
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07939671B2

反応ノート

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