Hydrochloric Acid → N-((6-chloropyridin-3-yl)methyl)-N-ethyl-2-methyl-4-nitro-8-oxa-2-aza-bicyclo[3.2.1]oct-3-en-3-amine

HRID 1043519ノート

反応式

HRID 1043519 の反応式
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][N:9]([CH2:17][CH3:18])[C:10]([NH:15][CH3:16])=[CH:11][N+:12]([O-:14])=[O:13])=[CH:4][CH:3]=1.[CH:19](=[O:24])[CH2:20][CH2:21][CH:22]=O.Cl>C(#N)C>[Cl:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][N:9]([CH2:17][CH3:18])[C:10]2[N:15]([CH3:16])[CH:22]3[O:24][CH:19]([C:11]=2[N+:12]([O-:14])=[O:13])[CH2:20][CH2:21]3)=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 12524ButanedialHCID 86457N-((6-Chloro-3-pyridinyl)methyl)-N-ethyl-N'-methyl-2-nitro-1,1-ethenediamine

生成物 1

HCID 58496253N-((6-chloropyridin-3-yl)methyl)-N-ethyl-2-methyl-4-nitro-8-oxa-2-aza-bicyclo[3.2.1]oct-3-en-3-amine収率 40%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a 50 ml round bottom flask was added 1.35 g (0.005 mol) N-((6-chloropyridin-3-yl)methyl)-N-ethyl-N′-methyl-2-nitroethene-1,1-diamine, 30 ml dry acetonitrile, 0.860 g (0.01 mol) succinaldehyde and catalytic concentrated HCl. The reaction was stirred at r.t. and monitored by TLC. After completion, the mixture was evaporated to remove solvent and purified by column chromatography to afford final product as faint yellow powder with 40% yield.

後処理

  1. customAfter completion, the mixture was evaporated
  2. customto remove solvent
  3. custompurified by column chromatography

出典と根拠

ORDレコード
ord-91bba571e5844645b9cdff758538430c
出典データセット
uspto-grants-2013_10
特許番号
US08563546B2

反応ノート

読み込み中…