3-Amino-6-chloro-4,5-dimethylpyridazine → HCID 71742687、化合物

HRID 1501344ノート

反応式

HRID 1501344 の反応式
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]

参加物

4

反応物 2

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

生成物 1

HCID 71742687HCID 71742687、化合物収率 49%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-e7bbc7c500d74f3ea9258285f2c94795
出典データセット
uspto-grants-2015_12
特許番号
US09206185B2

反応ノート

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