Triethylamine → 2-chloro-6-(5-cyclopropyl-1H-pyrazol-3-ylamino)-5-fluoro-4-iodonicotinonitrile

HRID 75938

반응식

HRID 75938 반응식
[Cl:1][C:2]1[N:9]=[C:8](Cl)[C:7]([F:11])=[C:6]([I:12])[C:3]=1[C:4]#[N:5].CCN(CC)CC.[CH:20]1([C:23]2[NH:27][N:26]=[C:25]([NH2:28])[CH:24]=2)[CH2:22][CH2:21]1>C(#N)C>[Cl:1][C:2]1[N:9]=[C:8]([NH:28][C:25]2[CH:24]=[C:23]([CH:20]3[CH2:22][CH2:21]3)[NH:27][N:26]=2)[C:7]([F:11])=[C:6]([I:12])[C:3]=1[C:4]#[N:5]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 27580143-cyclopropyl-1H-pyrazol-5-amineHCID 866206232,6-Dichloro-5-fluoro-4-iodonicotinonitrile

생성물 1

HCID 866206152-chloro-6-(5-cyclopropyl-1H-pyrazol-3-ylamino)-5-fluoro-4-iodonicotinonitrile수율 29.5%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
80 °C

실험 절차

The crude 2,6-dichloro-5-fluoro-4-iodonicotinonitrile (8.0 g, 25.2 mmol), Et3N (3.3 g, 32.8 mmol) and 5-cyclopropyl-1H-pyrazol-3-amine (3.1 g, 25.2 mmol) were placed in ACN (50 ml) and the resulting solution was heated to 80° C. for 24 hours. The reaction was cooled to room temperature, filtered, and the resulting solid was washed with cold ACN, dried, and collected to give the title compound (3.0 g, 29%). MS: Calcd.: 403. Found: [M+H]+ 404.

후처리

  1. temperatureThe reaction was cooled to room temperature
  2. filtrationfiltered
  3. washthe resulting solid was washed with cold ACN
  4. customdried
  5. customcollected

출처 및 근거

ORD 기록
ord-7fe79be0e3314cd9b2c9e39532c9b485
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08835465B2

연결된 노트

불러오는 중…