Acetic Anhydride → N'-(3-methyl-5-nitropyridin-2-yl)acetohydrazide

HRID 873918노트

반응식

HRID 873918 반응식
[NH:1]([C:3]1[C:8]([CH3:9])=[CH:7][C:6]([N+:10]([O-:12])=[O:11])=[CH:5][N:4]=1)[NH2:2].[CH3:13][C:14](OC(C)=O)=[O:15]>O1CCOCC1>[CH3:9][C:8]1[C:3]([NH:1][NH:2][C:14](=[O:15])[CH3:13])=[N:4][CH:5]=[C:6]([N+:10]([O-:12])=[O:11])[CH:7]=1

참가 물질

4

반응물 2

HCID 7918Acetic AnhydrideHCID 42361322-Hydrazinyl-3-methyl-5-nitropyridine

생성물 1

HCID 84818704N'-(3-methyl-5-nitropyridin-2-yl)acetohydrazide수율 100%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

To a suspension 2-hydrazinyl-3-methyl-5-nitropyridine (Step 67.1) (33.2 g, 198 mmol) in dioxane (175 mL) was added Ac2O (20.5 mL, 217 mmol) and the reaction was stirred at RT for min. The reaction mixture was poured onto ice-water and stirred for 1 hr at 0° C. The precipitate was collected by filtration, washed with H2O and Et2O, and dried under reduced pressure at 50° C. to afford the title product (41.5 g, 198 mmol, 99.5% yield) as light beige solid. tR: 0.45 min (LC-MS 2); ESI-MS: 211 [M+H]+; ESI-MS: 209 [M−H]− (LC-MS 2).

후처리

  1. additionThe reaction mixture was poured onto ice-water
  2. stirringstirred for 1 hr at 0° C
  3. filtrationThe precipitate was collected by filtration
  4. washwashed with H2O and Et2O
  5. customdried under reduced pressure at 50° C.

출처 및 근거

ORD 기록
ord-09bdcfece15d45468ded2e7d9a311ac3
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08975417B2

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