Pyridine → 6-Chloro-2-(ethylamino)pyridine-3-carbonyl fluoride

HRID 2088856노트

반응식

HRID 2088856 반응식
[Cl:1][C:2]1[N:7]=[C:6]([NH:8][CH2:9][CH3:10])[C:5]([C:11]([OH:13])=O)=[CH:4][CH:3]=1.N1C=CC=CC=1.N1C(F)=NC(F)=NC=1[F:22]>ClCCl>[Cl:1][C:2]1[N:7]=[C:6]([NH:8][CH2:9][CH3:10])[C:5]([C:11]([F:22])=[O:13])=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 1049PyridineHCID 12664Cyanuric fluorideHCID 633764796-Chloro-2-(ethylamino)nicotinic acid

생성물 1

HCID 867145746-Chloro-2-(ethylamino)pyridine-3-carbonyl fluoride수율 99%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a suspension of 10.5 g (52.3 mmol) of the compound obtained in step 1.1 in dichloromethane (250 ml) are successively added 4.2 ml (52.3 mmol) of pyridine and 8.4 ml (99.6 mmol) of cyanuric fluoride. The mixture is stirred for 3 hours at room temperature and then filtered. The solid is rinsed with dichloromethane (100 ml) and the filtrate is washed twice with ice-cold water (60 ml). The organic phase is dried over Na2SO4 and then concentrated under reduced pressure. 10.44 g of product are obtained, the form of an orange-coloured oil. Yield=99%. The product is used without purification in the following step.

후처리

  1. filtrationfiltered
  2. washThe solid is rinsed with dichloromethane (100 ml)
  3. washthe filtrate is washed twice with ice-cold water (60 ml)
  4. dry with materialThe organic phase is dried over Na2SO4
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-3e6fcac51b144091a84abeee34028be9
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08436011B2

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