3-Amino-6-chloro-4,5-dimethylpyridazine → HCID 71742687, 화합물

HRID 1501344노트

반응식

HRID 1501344 반응식
Cl[C:2]1[N:7]=[N:6][C:5]([NH2:8])=[C:4]([CH3:9])[C:3]=1[CH3:10].[CH3:11][O-:12].[Na+]>CO>[CH3:11][O:12][C:2]1[N:7]=[N:6][C:5]([NH2:8])=[C:4]([CH3:9])[C:3]=1[CH3:10]

참가 물질

4

반응물 2

HCID 69919433-Amino-6-chloro-4,5-dimethylpyridazineHCID 10942334Sodium Methoxide

생성물 1

HCID 71742687HCID 71742687, 화합물수율 49%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

6-Chloro-4,5-dimethylpyridazin-3-amine (CAS-Nr. 76593-36-7, 500 mg, 3.17 mmol, 1.0 eq) in 14.51 mL of a 25% solution (w/w) of sodium methylate in MeOH was heated for 1 h at 130° C. in a single mode microwave oven. The reaction mixture was partitioned between DCM and water. The organic phase was washed with brine and dried (Na2SO4 anh.). Volatile components were removed by the use of a rotary evaporator and the crude mixture was purified via MPLC (Biotage Isolera; 25 g SNAP NH2 cartridge: hexane→hexane/EtOAc 1/1) to give 250 mg (49% yield) of the title compound.

후처리

  1. customThe reaction mixture was partitioned between DCM and water
  2. washThe organic phase was washed with brine
  3. dry with materialdried (Na2SO4 anh.)
  4. customVolatile components were removed by the use of a rotary evaporator
  5. customthe crude mixture was purified via MPLC (Biotage Isolera; 25 g SNAP NH2 cartridge: hexane→hexane/EtOAc 1/1)

출처 및 근거

ORD 기록
ord-e7bbc7c500d74f3ea9258285f2c94795
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09206185B2

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