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Triethylamine → (2-Amino-4-methoxyphenyl)amide

HRID 2243349
ノート
印刷プレビュー

反応式

HRID 2243349 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[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:2]([O:34][CH:21]([CH3:20])[CH3:22])([CH3:7])[CH3:3].[NH2:10][C:3]1[CH:4]=[C:5]([O:8][CH3:9])[CH:6]=[CH:7][C:2]=1[NH-:1]
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 1534044-Methoxy-o-phenylenediamineHCID 87540947Fluoren-4-one-9-carboxylic acid chloride

生成物 2

HCID 7914Diisopropyl EtherHCID 86621037(2-Amino-4-methoxyphenyl)amide収率 124.9%

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 10 g of 1,2-diamino-4-methoxybenzene, 20 ml of triethylamine and 17 g of fluoren-4-one-9-carboxylic acid chloride in 600 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 6.2 g of (2-amino-4-methoxyphenyl)amide of 9-oxo-9H-fluorene-4-carboxylic acid, in the form of a brown 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-799ce49072ff449aa2a9213014e0f8e3
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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