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

HRID 2088856ノート

反応式

HRID 2088856 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3e6fcac51b144091a84abeee34028be9
出典データセット
uspto-grants-2013_05
特許番号
US08436011B2

反応ノート

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