Water → 6-Chloro-2-cyclopropylmethyl-2H-pyridazin-3-one

HRID 80951

반응식

HRID 80951 반응식
[CH:1]1([CH2:4]Br)[CH2:3][CH2:2]1.[Cl:6][C:7]1[CH:8]=[CH:9][C:10](=[O:13])[NH:11][N:12]=1.C([O-])([O-])=O.[K+].[K+].O>CN(C)C=O>[Cl:6][C:7]1[CH:8]=[CH:9][C:10](=[O:13])[N:11]([CH2:4][CH:1]2[CH2:3][CH2:2]2)[N:12]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 81503BromomethylcyclopropaneHCID 2528286-Chloropyridazin-3-ol

생성물 1

HCID 581095136-Chloro-2-cyclopropylmethyl-2H-pyridazin-3-one

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
60 °C

실험 절차

Cyclopropylmethyl bromide (0.82 mL) was added to a mixture of 6-chloro-2H-pyridazin-3-one (1.0 g) and K2CO3 (2.10 g) in N,N-dimethylformamide (10 mL). The resulting mixture was stirred at 60° C. overnight. Then, water was added and the mixture was extracted with ethyl acetate. The combined organic extracts were washed with water and brine and dried (MgSO4). After removal of the solvent, the residue was purified by chromatography on silica gel (CH2Cl2/MeOH/NH4OH 99:1:0.1) to afford the title compound as an oil.

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe combined organic extracts were washed with water and brine
  3. dry with materialdried (MgSO4)
  4. customAfter removal of the solvent
  5. customthe residue was purified by chromatography on silica gel (CH2Cl2/MeOH/NH4OH 99:1:0.1)

출처 및 근거

ORD 기록
ord-5c941b44a5f24da98bbb55349a3ff332
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846668B2

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