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Nitric Acid → 3-Bromo-2-methyl-7-nitrothieno[3,2-c]pyridin-4(5h)-one

HRID 1270849
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HRID 1270849 반응식
[N+:1]([O-:4])(O)=[O:2].[Br:5][C:6]1[C:10]2[C:11](=[O:15])[NH:12][CH:13]=[CH:14][C:9]=2[S:8][C:7]=1[CH3:16]>S(=O)(=O)(O)O.C1N(COCCO)C2NC(N)=NC(=O)C=2N=1>[Br:5][C:6]1[C:10]2[C:11](=[O:15])[NH:12][CH:13]=[C:14]([N+:1]([O-:4])=[O:2])[C:9]=2[S:8][C:7]=1[CH3:16]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 944Nitric AcidHCID 184507693-Bromo-2-methylthieno[3,2-c]pyridin-4(5H)-one

생성물 1

HCID 184507673-Bromo-2-methyl-7-nitrothieno[3,2-c]pyridin-4(5h)-one수율 106.8%

시약·촉매·용매 2

HCID 1118Sulfuric Acid용매HCID 178508935HCID 178508935, 화합물용매

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온도
0 °C

실험 절차

A solution of nitric acid (1.68 mL, 70%, 26. 8 mmol) in sulfuric acid (5 mL) was added dropwise to a 0° C. solution of Example 66A (3.27 g, 13.4 mmol) in sulfuric acic (15 mL). The resulting mixture was stirred at 0° C. for 1 hour, warmed to room temperature overnight, and poured into ice water. The resulting precipitate was collected by filtration, washed with water, and dried in a vacuum oven to provide 2.47 g (64% yield) of the desired product. MS (ESI(+)) m/e 290 (M+H)+.

후처리

  1. temperaturewarmed to room temperature overnight
  2. filtrationThe resulting precipitate was collected by filtration
  3. washwashed with water
  4. customdried in a vacuum oven

출처 및 근거

ORD 기록
ord-abe953ab24b64758b54fc830b9a8eca4
출처 데이터셋
uspto-grants-2007_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07202363B2

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