Potassium Carbonate → HCID 70206772、化合物

HRID 611567ノート

反応式

HRID 611567 の反応式
[ClH:1].Cl.[NH:3]1[CH2:7][CH2:6][CH2:5][C@H:4]1[C:8]1[O:16][C:11]2=[CH:12][N:13]=[CH:14][CH:15]=[C:10]2[CH:9]=1.[C:17]([O-])([O-])=O.[K+].[K+]>C(O)=O.C=O>[ClH:1].[ClH:1].[CH3:17][N:3]1[CH2:7][CH2:6][CH2:5][C@H:4]1[C:8]1[O:16][C:11]2=[CH:12][N:13]=[CH:14][CH:15]=[C:10]2[CH:9]=1

参加物

5

反応物 2

HCID 11430Potassium CarbonateHCID 70204345HCID 70204345、化合物

生成物 1

HCID 70206772HCID 70206772、化合物

試薬・触媒・溶媒 2

HCID 284Formic Acid溶媒HCID 712Formaldehyde溶媒

実験手順

A 120 mg sample of the compound from Example 9 above was dissolved in 4 mL of formic acid and 2 mL of formalin, and the reaction mixture was heated at reflux for 30 minutes. The reaction mixture was cooled to ambient temperature and poured into saturated K2CO3 solution. The resulting mixture was extracted with CH2Cl2, the extract was dried, and the solvent was removed. The residue was chromatographed on silica gel, and the compound was converted to the salt by treatment with HCl/ether: 1H NMR (D2O, 300 MHz) δ 2.30-2.40 (m, 3H), 2.50-2.74 (m, 1H), 2.98 (s, 3H), 3.45 (br d, 1H), 3.85 (br s, 1H), 4.97 (t, 1H), 7.47 (s, 1H), 8.08 (d, 1H), 8.51 (d, 1H), 9.10 (s, 1H); MS m/z: 203 (M+H)+ ; Anal. Calcd for C12H14N2O·2 HCl.0.5H2O: C, 50.70; H, 6.03; N, 9.86. Found: C, 50.69; H, 6.09; N, 9.61.

後処理

  1. temperatureat reflux for 30 minutes
  2. extractionThe resulting mixture was extracted with CH2Cl2
  3. customthe extract was dried
  4. customthe solvent was removed
  5. customThe residue was chromatographed on silica gel

出典と根拠

ORDレコード
ord-034acf24d6cb41bfb4ce2ca6f420c28d
出典データセット
uspto-grants-1999_12
特許番号
US06001849

反応ノート

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