1,2-Dichloroethane → 4-bromo-1,3-dimethyl-1H-pyrazole-5-carboxamide

HRID 58061

反応式

HRID 58061 の反応式
[Br:1][C:2]1[C:3]([CH3:11])=[N:4][N:5]([CH3:10])[C:6]=1[C:7](O)=[O:8].[Cl-].[NH4+].C1C=CC2N(O)N=[N:20]C=2C=1.C(Cl)CCl.C(N(C(C)C)C(C)C)C>CN(C=O)C.CCOC(C)=O>[Br:1][C:2]1[C:3]([CH3:11])=[N:4][N:5]([CH3:10])[C:6]=1[C:7]([NH2:20])=[O:8]

参加物

8

反応物 5

HCID 111,2-DichloroethaneHCID 25517Ammonium ChlorideHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 27798334-bromo-1,3-dimethyl-1H-pyrazole-5-carboxylic acid

生成物 1

HCID 47661424-bromo-1,3-dimethyl-1H-pyrazole-5-carboxamide

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To 4-bromo-1,3-dimethyl-1H-pyrazole-5-carboxylic acid (0.3 g, 1.370 mmol) in DMF (5 mL) were added ammonium chloride (0.293 g, 5.48 mmol), HOBt (0.222 g, 1.644 mmol), and EDC (0.368 g, 1.917 mmol), followed by N-ethyl-N-isopropylpropan-2-amine (1.193 mL, 6.85 mmol). The reaction mixture was stirred for 18 hours at room temperature. The reaction mixture was subsequently diluted with EtOAc, washed with brine, dried over Na2SO4, and concentrated to give the title compound, which was used without further purification (0.28 g).

後処理

  1. washwashed with brine
  2. dry with materialdried over Na2SO4
  3. concentrationconcentrated

出典と根拠

ORDレコード
ord-cc234f99af78493bbb90bc9a27ab3330
出典データセット
uspto-grants-2016_09
特許番号
US09434743B2

関連ノート

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