Water → N,N-Dimethyl-1H-indazole-3-carboxamide

HRID 240798

반응식

HRID 240798 반응식
[NH:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3]([C:10]([OH:12])=O)=[N:2]1.C(C1NC=CN=1)([C:15]1[NH:16][CH:17]=CN=1)=O.Cl.CNC.O>CN(C)C=O>[CH3:15][N:16]([CH3:17])[C:10]([C:3]1[C:4]2[C:9](=[CH:8][CH:7]=[CH:6][CH:5]=2)[NH:1][N:2]=1)=[O:12]

참가 물질

6

반응물 4

HCID 962WaterHCID 10473Dimethylamine, hydrochlorideHCID 78250Indazole-3-carboxylic acidHCID 5250894Bis-(1H-imidazol-2-YL)-methanone

생성물 1

HCID 20816326N,N-Dimethyl-1H-indazole-3-carboxamide

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
60 °C

실험 절차

1H-Indazole-3-carboxylic acid (5.0 g, 30.8 mmol) and carbonyl diimidazole (5.0 g, 33.9 mmol) were dissolved in N,N-dimethylformamide (150 mL) and heated to 60° C. After 2 hours, dimethylamine hydrochloride (4.0 g, 33.9) was added, and the reaction was stirred for an additional hour at 60° C. The reaction was poured into water, and the aqueous phase was extracted with ethyl acetate (3×150 mL). The combined organic phases were washed sequentially with aqueous sodium bicarbonate, 10% hydrochloric acid, water and brine. After drying over magnesium sulfate, filtering and concentrating in vacuo, the title compound was obtained.

후처리

  1. extractionthe aqueous phase was extracted with ethyl acetate (3×150 mL)
  2. washThe combined organic phases were washed sequentially with aqueous sodium bicarbonate, 10% hydrochloric acid, water and brine
  3. dry with materialAfter drying over magnesium sulfate
  4. filtrationfiltering
  5. concentrationconcentrating in vacuo

출처 및 근거

ORD 기록
ord-8e15ba4e94764231a73f3a5ba168eef4
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08648069B2

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