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

HRID 58061

반응식

HRID 58061 반응식
[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]

참가 물질

8

반응물 5

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

생성물 1

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

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-cc234f99af78493bbb90bc9a27ab3330
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09434743B2

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