Hydrochloric Acid → 6-Methoxypyridine-2-carbohydrazide

HRID 1889034노트

반응식

HRID 1889034 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 242291726-Methoxypyridine-2-carbohydrazide수율 167.1%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-fca7ee8762b7489288c9e161dcee6b74
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08501946B2

반응 노트

불러오는 중…