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HCID 57781108, 화합물 → HCID 57781121, 화합물

HRID 1690722
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HRID 1690722 반응식
[C:1]([C:4]1[N:8]([CH:9]2[C:18]3[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=3)[C:12](=[O:19])[O:11][C:10]2([CH3:21])[CH3:20])[CH:7]=[N:6][CH:5]=1)([CH3:3])=[CH2:2]>CO.[Pd]>[CH:1]([C:4]1[N:8]([CH:9]2[C:18]3[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=3)[C:12](=[O:19])[O:11][C:10]2([CH3:21])[CH3:20])[CH:7]=[N:6][CH:5]=1)([CH3:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 57781108HCID 57781108, 화합물

생성물 1

HCID 57781121HCID 57781121, 화합물수율 92.7%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

To a solution of 4-(5-isopropenyl-imidazol-1-yl)-3,3-dimethyl-isochroman-1-one (0.225 g, 0.797 mmol) (Example 4) in methanol (5 mL) is added Pd/C (0.250 g). The reaction vessel is flushed with hydrogen gas and stirred under balloon pressure for 72 h. The mixture is filtered and the filtrate concentrated in vacuo to give a 4-(5-isopropyl-imidazol-1-yl)-3,3-dimethyl-isochroman-1-one(0.210 g) as yellow solid (ESI) m/z 285.0 (M+H); 1H NMR (400 MHz, MeOD) δ ppm 1.24 (s, 3 H), 1.41 (d, J=6.6 Hz, 3 H), 1.45 (d, J=6.8 Hz, 3 H), 1.56 (s, 3H), 3.23 (br. s, 1 H), 5.60 (br. s, 1 H), 6.88 (br. s, 1 H), 7.15 (br. s, 1 H), 7.44 (d, J=7.3 Hz, 1H), 7.68 (td, J=7.6, 1.1 Hz, 1 H), 7.79 (td, J=7.6, 1.3 Hz, 1 H), 8.25 (dd, J=7.8, 1.3 Hz, 1 H).

후처리

  1. customThe reaction vessel is flushed with hydrogen gas
  2. filtrationThe mixture is filtered
  3. concentrationthe filtrate concentrated in vacuo

출처 및 근거

ORD 기록
ord-d4e77911eb5e4f699fc0a9a0412ec9f9
출처 데이터셋
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08153674B2

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