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Sodium Carbonate → N-[2-(4-nitro-2-methylphenylamino)ethyl]-2,2,2-trifluoroacetamide

HRID 970235
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HRID 970235 반응식
F[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[CH3:11].C(=O)([O-])[O-].[Na+].[Na+].Cl.[F:19][C:20]([F:28])([F:27])[C:21]([NH:23][CH2:24][CH2:25][NH2:26])=[O:22].CN1CCCC1=O>O>[N+:8]([C:5]1[CH:6]=[CH:7][C:2]([NH:26][CH2:25][CH2:24][NH:23][C:21](=[O:22])[C:20]([F:28])([F:27])[F:19])=[C:3]([CH3:11])[CH:4]=1)([O-:10])=[O:9]
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참가 물질

6

반응물 4

HCID 10340Sodium CarbonateHCID 13387N-methyl-2-pyrrolidoneHCID 68001Benzene, 1-fluoro-2-methyl-4-nitro-HCID 23021610N-(2-aminoethyl)-2,2,2-trifluoroacetamide hydrochloride

생성물 1

HCID 23104329N-[2-(4-nitro-2-methylphenylamino)ethyl]-2,2,2-trifluoroacetamide수율 65.2%

시약·촉매·용매 1

HCID 962
Water
용매

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온도
90 °C

실험 절차

1.55 g (0.01 mol) of 2-fluoro-5-nitrotoluene, 2.65 g (0.025 mol) of sodium carbonate, 2.11 g (0.011 mol) of 2-(trifluoroacetamido)ethylamine hydrochloride and 10 ml of N-methyl-pyrrolidone were introduced into a three-necked flask under nitrogen. The mixture was heated to 90° C. After reaction for 48 hours, the reaction mixture was cooled and 30 ml of distilled water were then added slowly with vigorous stirring. A yellow precipitate appeared. This precipitate was filtered off, washed several times with water and then with pentane, and dried under vacuum. 1.9 g of expected nitro derivative (1) were obtained in the form of a yellow powder.

후처리

  1. customAfter reaction for 48 hours
  2. temperaturethe reaction mixture was cooled
  3. filtrationThis precipitate was filtered off
  4. washwashed several times with water
  5. dry with materialwith pentane, and dried under vacuum

출처 및 근거

ORD 기록
ord-30b2ebf634ba4af2924cdcd55c2bb20e
출처 데이터셋
uspto-grants-2007_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07311737B2

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