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Triethylamine → (2-Amino-4,5-difluorophenyl)amide

HRID 2243344
ノート
印刷プレビュー

反応式

HRID 2243344 の反応式
[NH2:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([F:9])=[CH:4][C:3]=1[NH2:10].C(N(CC)CC)C.C1C=[CH:20][C:21](=[O:34])[C:22]2C=1C(C(Cl)=O)=C1C=2C=CC=C1>ClCCl>[CH:21]([O:34][CH:7]([CH3:6])[CH3:2])([CH3:22])[CH3:20].[NH2:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([F:9])=[CH:4][C:3]=1[NH-:10]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 8471TriethylamineHCID 27367551,2-Diamino-4,5-difluorobenzeneHCID 87540947Fluoren-4-one-9-carboxylic acid chloride

生成物 2

HCID 7914Diisopropyl EtherHCID 131727951(2-Amino-4,5-difluorophenyl)amide収率 282%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane
溶媒

実験手順

The procedure used in stage 1 of Example 1 is followed, but starting from 1 g of 1,2-diamino-4,5-difluorobenzene, 1.9 ml of triethylamine and 1.7 g of fluoren-4-one-9-carboxylic acid chloride in 50 ml of dichloromethane. After stirring for 20 hours at room temperature, the precipitate that formed is filtered off, and washed with dichloromethane, with water, then with a 10% saturated aqueous solution of sodium hydrogen carbonate and, finally, with water. After formation of a paste with diisopropyl ether, in this way we obtain 1.4 g of (2-amino-4,5-difluorophenyl)amide of 9-oxo-9H-fluorene-4-carboxylic acid, in the form of a yellow powder, which is used as it is in the following stage, with the following characteristics:

後処理

  1. customthe precipitate that formed
  2. filtrationis filtered off
  3. washwashed with dichloromethane, with water

出典と根拠

ORDレコード
ord-6fd5fc1458594209aa813a02f885044f
出典データセット
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07674795B2

反応ノート

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