HCID 59520005, 화합물 → HCID 53402950, 화합물

HRID 1162081노트

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HRID 1162081 반응식
[Br:1][C:2]1[CH:3]=[C:4]([N+:14]([O-:16])=[O:15])[C:5]2[O:9][CH:8]=[C:7](C(O)=O)[C:6]=2[CH:13]=1>N1C2C(=CC=CC=2)C=CC=1.C1(C)C=CC=CC=1>[Br:1][C:2]1[CH:3]=[C:4]([N+:14]([O-:16])=[O:15])[C:5]2[O:9][CH:8]=[CH:7][C:6]=2[CH:13]=1

참가 물질

4

반응물 1

HCID 59520005HCID 59520005, 화합물

생성물 1

HCID 53402950HCID 53402950, 화합물

시약·촉매·용매 2

HCID 1140Toluene용매HCID 7047Quinoline용매

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온도
190 °C

실험 절차

5-Bromo-7-nitro-1-benzofuran-3-carboxylic acid (4.65 g, 16 mmol; obtained in Step 2) was suspended in quinoline (25 mL), 0.1 g CuO was added and the mixture heated to 190° C. for 30 minutes. The warm reaction mixture was diluted with hot toluene (100 mL), filtered and the filter cake washed with hot toluene (total 400 mL). The combined toluene extracts were washed with 1 M HCl (2×100 mL) and brine, evaporated and the solid product washed with hexane, collected by filtration and dried. Yield: 1.9 g (48%). 1H NMR (400 MHz, DMSO-d6) δ ppm 7.13 (d, J=2.3 Hz, 1H) 8.20 (d, J=2.0 Hz, 1H) 8.28 (d, J=2.3 Hz, 1H) 8.32 (d, J=2.0 Hz, 1H).

후처리

  1. customThe warm reaction mixture
  2. filtrationfiltered
  3. washthe filter cake washed with hot toluene (total 400 mL)
  4. washThe combined toluene extracts were washed with 1 M HCl (2×100 mL) and brine
  5. customevaporated
  6. washthe solid product washed with hexane
  7. filtrationcollected by filtration
  8. customdried

출처 및 근거

ORD 기록
ord-2329a03cd50e498ca1c297c3280369e9
출처 데이터셋
uspto-grants-2010_10
특허 번호
US07820675B2

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