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Water → 2-trifluoromethyl-nicotinic acid N'-(3,4-dimethoxy-5-nitro-benzoyl)-hydrazide

HRID 1920062
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HRID 1920062 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:9]=[C:10]([N+:14]([O-:16])=[O:15])[C:11]=1[O:12][CH3:13])[C:6]([OH:8])=O.[F:17][C:18]([F:30])([F:29])[C:19]1[N:28]=[CH:27][CH:26]=[CH:25][C:20]=1[C:21]([NH:23][NH2:24])=[O:22].O>O1CCCC1>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:9]=[C:10]([N+:14]([O-:16])=[O:15])[C:11]=1[O:12][CH3:13])[C:6]([NH:24][NH:23][C:21](=[O:22])[C:20]1[CH:25]=[CH:26][CH:27]=[N:28][C:19]=1[C:18]([F:17])([F:29])[F:30])=[O:8]
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참가 물질

5

반응물 3

HCID 962WaterHCID 219286243,4-Dimethoxy-5-nitrobenzoic acidHCID 670371942-(Trifluoromethyl)pyridine-3-carbohydrazide

생성물 1

HCID 670371772-trifluoromethyl-nicotinic acid N'-(3,4-dimethoxy-5-nitro-benzoyl)-hydrazide

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of 3,4-dimethoxy-5-nitrobenzoic acid (0.53 g, 2.34 mmol) and 1,1-carbonyldiimidazole (0.42 g, 2.59 mmol) was heated in tetrahydrofuran (10 mL) at reflux for three hours and then cooled to room temperature. 2-Trifluoromethyl-nicotinic acid hydrazide (0.53 g, 2.57 mmol) was added in one portion and the yellowish mixture was stirred at reflux overnight and then allowed to cool to room temperature. The mixture was poured onto cold water (100 mL) and the copious precipitate was filtered off, washed with water and dried to give 2-trifluoromethyl-nicotinic acid N′-(3,4-dimethoxy-5-nitro-benzoyl)-hydrazide, 0.71 g (73%).

후처리

  1. temperatureat reflux for three hours
  2. temperatureat reflux overnight
  3. temperatureto cool to room temperature
  4. filtrationthe copious precipitate was filtered off
  5. washwashed with water
  6. customdried

출처 및 근거

ORD 기록
ord-34e15dbf768e4e38bfaa7abdb369acf7
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08168793B2

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