HCID 59520005、化合物 → HCID 53402950、化合物

HRID 1162081ノート

反応式

HRID 1162081 の反応式
[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

参加物

4

反応物 1

HCID 59520005HCID 59520005、化合物

生成物 1

HCID 53402950HCID 53402950、化合物

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 7047Quinoline溶媒

反応条件

温度
190 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-2329a03cd50e498ca1c297c3280369e9
出典データセット
uspto-grants-2010_10
特許番号
US07820675B2

反応ノート

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