甲苯 → Methyl4-[4-(methylamino)-3-nitrophenoxy]pyridine-3-carboxylate

HRID 13503

反应方程式

HRID 13503 反应方程式
COC([C:5]1C=N[CH:8]=[C:9]([O:11][C:12]2[CH:17]=[CH:16][C:15]([NH:18][C:19](=O)C(F)(F)F)=[C:14]([N+:25]([O-:27])=[O:26])[CH:13]=2)[CH:10]=1)=O.[C:28](#[N:30])C.[OH-:31].[Na+].S(OC)([O:36][CH3:37])(=O)=O.[C:40]1(C)C=CC=CC=1>[Cl-].C([N+](C)(C)C)C1C=CC=CC=1>[CH3:40][O:31][C:37]([C:8]1[CH:28]=[N:30][CH:5]=[CH:10][C:9]=1[O:11][C:12]1[CH:17]=[CH:16][C:15]([NH:18][CH3:19])=[C:14]([N+:25]([O-:27])=[O:26])[CH:13]=1)=[O:36]

参与物

7

反应物 5

HCID 1140甲苯HCID 6342乙腈HCID 6497甲基硫酸酯-13C2HCID 14798二甲基对苯二胺二盐酸HCID 22040901Methyl5-[3-nitro-4-(2,2,2-trifluoroacetylamino)phenoxy]-pyridine-3-carboxylate

产物 1

HCID 22040570Methyl4-[4-(methylamino)-3-nitrophenoxy]pyridine-3-carboxylate

试剂、催化剂与溶剂 1

HCID 5963苄基三甲基氯化铵催化剂

实验过程

To the solution of the methyl5-[3-nitro-4-(2,2,2-trifluoroacetylamino)phenoxy]-pyridine-3-carboxylate (1 eq) in a mixture of toluene, acetonitrile and sodium hydroxide solution (50%) was added benzyltrimethylammonium chloride (1 eq) and dimethyl sulfate (1.2 eq). The biphasic mixture was stirred overnight at room temperature and evaporated. The mixture was taken up in ethyl acetate, washed with water, brine, dried and evaporated. The crude was purified by column chromatography to afford methyl-4-[4-(methylamino)-3-nitrophenoxy]pyridine-3-carboxylate. MS: MH+=303.

后处理

  1. customevaporated
  2. washwashed with water, brine
  3. customdried
  4. customevaporated
  5. customThe crude was purified by column chromatography

来源与证据

ORD记录
ord-bf6dc933770b47d2a8ca9040f0f8e650
来源数据集
uspto-grants-2010_06
专利号
US07728010B2

关联笔记

加载中…