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

HRID 873918ノート

反応式

HRID 873918 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

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).

後処理

  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.

出典と根拠

ORDレコード
ord-09bdcfece15d45468ded2e7d9a311ac3
出典データセット
uspto-grants-2015_03
特許番号
US08975417B2

反応ノート

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