Water → N,N-Diethyl-3,6-dichloropyridazine-4-carboxamide

HRID 1524517노트

반응식

HRID 1524517 반응식
[Cl:1][C:2]1[N:3]=[N:4][C:5]([Cl:11])=[CH:6][C:7]=1[C:8](Cl)=[O:9].[CH2:12]([NH:14][CH2:15][CH3:16])[CH3:13].O>C(Cl)Cl>[CH2:12]([N:14]([CH2:15][CH3:16])[C:8]([C:7]1[CH:6]=[C:5]([Cl:11])[N:4]=[N:3][C:2]=1[Cl:1])=[O:9])[CH3:13]

참가 물질

5

반응물 3

HCID 962WaterHCID 8021DiethylamineHCID 810183,6-Dichloropyridazine-4-carbonyl chloride

생성물 1

HCID 58136931N,N-Diethyl-3,6-dichloropyridazine-4-carboxamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

3,6-Dichloropyridazine-4-carbonyl chloride (2.5 g) was initially charged in DCM (25 ml) at RT. Thereafter, diethylamine (1.5 ml) predissolved in DCM (5 ml) was slowly added dropwise while stirring. After stirring at RT for 3 h, the mixture was admixed with water and extracted three times with DCM. The combined DCM phases were dried over sodium sulfate, filtered and concentrated. The residue was purified by means of silica gel (70 g cartridge, n-heptane/EA gradient). 1.8 g of the title compound were obtained.

후처리

  1. additionwas slowly added dropwise
  2. stirringAfter stirring at RT for 3 h
  3. extractionextracted three times with DCM
  4. dry with materialThe combined DCM phases were dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe residue was purified by means of silica gel (70 g cartridge, n-heptane/EA gradient)

출처 및 근거

ORD 기록
ord-2f2ece0aaeb0473e96d5f12e5cc7cdce
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09079906B2

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