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

HRID 1696754노트

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HRID 1696754 반응식
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

참가 물질

4

반응물 2

HCID 714642286-Bromo-4-methoxypyridin-2-amineHCID 178418546HCID 178418546, 화합물

생성물 1

HCID 552848206-Amino-4-methoxypicolinonitrile수율 29.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
220 °C

실험 절차

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

후처리

  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

출처 및 근거

ORD 기록
ord-8ce4d24ff6b14d868002dbdb90171ead
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08163778B2

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