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HCID 68521328, 화합물 → HCID 57850280, 화합물

HRID 736661
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HRID 736661 반응식
[CH2:1]([O:3][C:4](/[CH:6]=[C:7]1/[C:8]([CH3:21])([CH3:20])[CH2:9][N:10]([C:13]([O:15][C:16]([CH3:19])([CH3:18])[CH3:17])=[O:14])[CH2:11][CH2:12]/1)=[O:5])[CH3:2]>CO.[Pd]>[CH2:1]([O:3][C:4]([CH2:6][CH:7]1[CH2:12][CH2:11][N:10]([C:13]([O:15][C:16]([CH3:19])([CH3:18])[CH3:17])=[O:14])[CH2:9][C:8]1([CH3:20])[CH3:21])=[O:5])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 68521328HCID 68521328, 화합물

생성물 1

HCID 57850280HCID 57850280, 화합물수율 68.3%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

A solution of (E)-tert-butyl 4-{(ethoxycarbonyl)methylene}-3,3-dimethylpiperidine-1-carboxylate (784 mg, 2.64 mmol) in MeOH (10 mL) containing Pd/C (131 mg) was hydrogenated at 1 atm. After 10 h, the mixture was filtered, and the filter cake was washed with MeOH. The combined filtrates were concentrated to afford the titled compound (540 mg, 68%): 1H NMR (CDCl3) δ 4.13 (q, J=6.8 Hz, 2H), 4.05 (m, 1H), 3.57 (m, 1H), 2.57 (m, 1H), 2.46 (dd, J=15.2, 3.2 Hz, 1H), 1.93 (dd, J=15.2, 10.4 Hz, 1H), 1.76 (m, 1H), 1.59-1.50 (m, 2H), 1.45 (s, 9H) 1.34 (m, 1H), 1.26 (t, J=6.8 Hz, 3H), 0.91 (s, 3H), 0.79 (s, 3H).

후처리

  1. filtrationthe mixture was filtered
  2. washthe filter cake was washed with MeOH
  3. concentrationThe combined filtrates were concentrated

출처 및 근거

ORD 기록
ord-228f885fdd60400b89204791f135c168
출처 데이터셋
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07595401B2

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