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Acetic Anhydride → HCID 73031688, 화합물

HRID 1663299
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HRID 1663299 반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([CH:7]=[N:8][N:9]2[CH2:18][C:17]3[C:12](=[CH:13][CH:14]=[C:15]([C:19]([F:28])([C:24]([F:27])([F:26])[F:25])[C:20]([F:23])([F:22])[F:21])[CH:16]=3)[NH:11][C:10]2=[O:29])[CH:2]=1.[H-].[Na+].[C:32](OC(=O)C)(=[O:34])[CH3:33]>CC(N(C)C)=O>[C:32]([N:11]1[C:12]2[C:17](=[CH:16][C:15]([C:19]([F:28])([C:24]([F:25])([F:26])[F:27])[C:20]([F:22])([F:21])[F:23])=[CH:14][CH:13]=2)[CH2:18][N:9]([N:8]=[CH:7][C:3]2[CH:2]=[N:1][CH:6]=[CH:5][CH:4]=2)[C:10]1=[O:29])(=[O:34])[CH3:33]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7918Acetic AnhydrideHCID 24758Sodium hydrideHCID 730165883,4-dihydro-3-(3-pyridylmethylideneamino)-6-[1,2,2,2-tetrafluoro-1-(trifluoromethyl)ethyl]-2(1H)-quinazolinone

생성물 1

HCID 73031688HCID 73031688, 화합물수율 93.7%

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

실험 절차

In 10 ml of dimethylacetamide was dissolved 0.84 g (1.8 mmol) of 3-(3-pyridylmethylideneamino)-3,4-dihydro-6-[1,2,2,2-tetrafluoro-1-(trifluoromethyl)ethyl]-2(1H)-quinazolinone, and to the resulting solution was added 0.09 g (2.3 mmol) of sodium hydride (purity: 62.4%). The reaction was carried out at room temperature for 30 minutes, after which 0.25 g (2.4 mmol) of acetic anhydride was added and the reaction was carried out for 4 hours. After completion of the reaction, the reaction solution was poured into ice water and the desired compound was extracted with ethyl acetate (20 ml×3). The extract solution was washed with water and saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and then concentrated in vacuo. The crude product thus obtained was purified by silica gel column chromatography (ethyl acetate−methanol=10:1) to obtain 0.78 g of the desired compound.

후처리

  1. waitthe reaction was carried out for 4 hours
  2. customAfter completion of the reaction
  3. extractionthe desired compound was extracted with ethyl acetate (20 ml×3)
  4. washThe extract solution was washed with water and saturated aqueous sodium chloride solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated in vacuo
  7. customThe crude product thus obtained
  8. customwas purified by silica gel column chromatography (ethyl acetate−methanol=10:1)

출처 및 근거

ORD 기록
ord-ec75481853414e9c95bd9ae8da094b36
출처 데이터셋
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08034931B2

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