HCID 18762004, 화합물 → HCID 69905062, 화합물

HRID 430903노트

반응식

HRID 430903 반응식
[CH3:1][N:2]1[CH2:6][CH2:5][CH2:4][CH:3]1[C:7]1[CH:8]=[C:9]([C:13]#[C:14][C:15]2[CH:24]=[CH:23][C:18]([C:19]([O:21][CH3:22])=[O:20])=[CH:17][CH:16]=2)[CH:10]=[N:11][CH:12]=1>CO>[CH3:1][N:2]1[CH2:6][CH2:5][CH2:4][CH:3]1[C:7]1[CH:12]=[N:11][CH:10]=[C:9]([CH2:13][CH2:14][C:15]2[CH:16]=[CH:17][C:18]([C:19]([O:21][CH3:22])=[O:20])=[CH:23][CH:24]=2)[CH:8]=1

참가 물질

3

반응물 1

HCID 18762004HCID 18762004, 화합물

생성물 1

HCID 69905062HCID 69905062, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of YH19 (0.15 g, 0.468 mmol) and Pd(C) (10%, 20 mg) in MeOH (10 mL) was hydrogenated at atmospheric pressure and room temperature for one day. The catalyst was removed by filtration through Celite and the filtrate was concentrated. The residue was chromatographed [SiO2, CHCl3/MeOH (60:1)] to give 0.15 g (95%) of YH22; 1H NMR (400 MHz, CDCl3) δ 8.38 (br s, 2H), 7.91-7.80 (m, 2H), 7.40 (s, 1H), 7.16-7.14 (m, 2H), 3.85 (s, 3H), 3.23-3.16 (m, 1H), 3.05-2.87 (m, 5H), 2.30-2.22 (m, 1H), 2.18-2.08 (m, 1H), 2.09 (s, 3H), 1.92-1.84 (m, 1H), 1.81-1.72 (m, 1H), 1.67-1.57 (m, 1H); 13C NMR (400 MHz, CDCl3) δ 166.9, 148.6, 147.3, 146.2, 138.3, 136.5, 134.5, 129.7, 128.0, 68.6, 56.9, 51.9, 40.2, 37.4, 35.0, 34.4, 22.4;

후처리

  1. customThe catalyst was removed by filtration through Celite
  2. concentrationthe filtrate was concentrated
  3. customThe residue was chromatographed [SiO2, CHCl3/MeOH (60:1)]
  4. customto give 0.15 g (95%) of YH22

출처 및 근거

ORD 기록
ord-30ee736460c943088a8e7d2681e63854
출처 데이터셋
uspto-grants-2003_12
특허 번호
US06656469B1

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