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

HRID 2243329
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HRID 2243329 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][C:9]([F:12])([F:11])[F:10])=[CH:4][C:3]=1[NH2:13].C(N(CC)CC)C.C1C=[CH:23][C:24](=[O:37])[C:25]2C=1C(C(Cl)=O)=C1C=2C=CC=C1>ClCCl>[CH:2]([O:37][CH:24]([CH3:23])[CH3:25])([CH3:7])[CH3:3].[NH2:13][C:3]1[CH:4]=[C:5]([O:8][C:9]([F:10])([F:11])[F:12])[CH:6]=[CH:7][C:2]=1[NH-:1]
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참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 27739594-(Trifluoromethoxy)benzene-1,2-diamineHCID 87540947Fluoren-4-one-9-carboxylic acid chloride

생성물 2

HCID 7914Diisopropyl EtherHCID 86621031(2-Amino-4-trifluoromethoxyphenyl)amide수율 97.5%

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

실험 절차

The procedure used in stage 1 of Example 1 is followed, but starting from 1 g of 1,2-diamino-4-(trifluoromethoxy)benzene, 1.3 ml of triethylamine and 1.15 g of fluoren-4-one-9-carboxylic acid chloride in 30 ml of dichloromethane. After stirring for 20 hours at room temperature, the precipitate that formed is filtered off, and washed with dichloromethane, with water, and then with a 10% saturated aqueous solution of sodium hydrogen carbonate and, finally, with water. After drying and formation of a paste with diisopropyl ether, in this way we obtain 485 mg of (2-amino-4-trifluoromethoxyphenyl)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:

후처리

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

출처 및 근거

ORD 기록
ord-a6bb55ee8db14c528feb4c4249da5423
출처 데이터셋
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07674795B2

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