Hydrochloric Acid → 6-Methoxypyridine-2-carbohydrazide

HRID 1889034ノート

反応式

HRID 1889034 の反応式
[CH3:1][O:2][C:3]1[N:8]=[C:7]([C:9]([NH:11][NH:12]C(OC(C)(C)C)=O)=[O:10])[CH:6]=[CH:5][CH:4]=1.Cl>O1CCOCC1>[CH3:1][O:2][C:3]1[N:8]=[C:7]([C:9]([NH:11][NH2:12])=[O:10])[CH:6]=[CH:5][CH:4]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 665988541,1-Dimethylethyl 2-{[6-(methyloxy)-2-pyridinyl]carbonyl}hydrazinecarboxylate

生成物 1

HCID 242291726-Methoxypyridine-2-carbohydrazide収率 167.1%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

1,1-dimethylethyl 2-{[6-(methyloxy)-2-pyridinyl]carbonyl}hydrazinecarboxylate (194)(1.685 g, 6.30 mmol) was dissolved in 1,4-dioxane (21.01 ml) and HCl (4M in 1,4-dioxane) (15.76 ml, 63.0 mmol) was added. The solution was stirred at room temperature for 5 hours. LCMS showed that no starting material remained and the product had formed. The solvent was removed under reduced pressure to afford 1.76 g of the crude material. The crude material was loaded onto two 10 g SCX columns and these were washed with methanol. The product was eluted off using 2M ammonia in methanol and the solvent was removed under reduced pressure to afford the purified desired product in 0.954 g.

後処理

  1. customthe product had formed
  2. customThe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-fca7ee8762b7489288c9e161dcee6b74
出典データセット
uspto-grants-2013_08
特許番号
US08501946B2

反応ノート

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