Potassium Carbonate → HCID 70206772, 화합물

HRID 611567노트

반응식

HRID 611567 반응식
[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

참가 물질

5

반응물 2

HCID 11430Potassium CarbonateHCID 70204345HCID 70204345, 화합물

생성물 1

HCID 70206772HCID 70206772, 화합물

시약·촉매·용매 2

HCID 284Formic Acid용매HCID 712Formaldehyde용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-034acf24d6cb41bfb4ce2ca6f420c28d
출처 데이터셋
uspto-grants-1999_12
특허 번호
US06001849

반응 노트

불러오는 중…