6-Bromo-4-methoxypyridin-2-amine → 6-Amino-4-methoxypicolinonitrile

HRID 1696754ノート

反応式

HRID 1696754 の反応式
Br[C:2]1[N:7]=[C:6]([NH2:8])[CH:5]=[C:4]([O:9][CH3:10])[CH:3]=1.[Cu][C:12]#[N:13]>CN(C)C=O>[NH2:8][C:6]1[N:7]=[C:2]([C:12]#[N:13])[CH:3]=[C:4]([O:9][CH3:10])[CH:5]=1

参加物

4

反応物 2

HCID 714642286-Bromo-4-methoxypyridin-2-amineHCID 178418546HCID 178418546、化合物

生成物 1

HCID 552848206-Amino-4-methoxypicolinonitrile収率 29.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
220 °C

実験手順

To a solution of 0.40 g 6-bromo-4-methoxy-pyridin-2-ylamine in 8.0 ml dimethylformamide was added 0.265 g copper(I) cyanide and the mixture was heated to 220° C. under microwave irradiation for 6 min. The reaction mixture was partitioned between water and ethyl acetate. The phases were separated and washed with water and brine, dried over magnesium sulfate dihydrate and purified by chromatography on silica gel with heptane : ethyl acetate to yield 0.086 g of the title compound as greenish solid MS (ISP) M+H+=183.1

後処理

  1. customThe reaction mixture was partitioned between water and ethyl acetate
  2. customThe phases were separated
  3. washwashed with water and brine
  4. dry with materialdried over magnesium sulfate dihydrate
  5. custompurified by chromatography on silica gel with heptane

出典と根拠

ORDレコード
ord-8ce4d24ff6b14d868002dbdb90171ead
出典データセット
uspto-grants-2012_04
特許番号
US08163778B2

反応ノート

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