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HCID 72465841, 화합물 → HCID 69367981, 화합물

HRID 851956
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HRID 851956 반응식
[CH2:1]([O:3][C:4](=[O:34])[CH:5]([N:20]=C(C1C=CC=CC=1)C1C=CC=CC=1)[CH2:6][CH2:7][C:8]([C:10]1[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[C:12]([CH3:18])[C:11]=1[CH3:19])=O)[CH3:2]>CCO.[Pd]>[CH2:1]([O:3][C:4]([C@H:5]1[CH2:6][CH2:7][C@@H:8]([C:10]2[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[C:12]([CH3:18])[C:11]=2[CH3:19])[NH:20]1)=[O:34])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 72465841HCID 72465841, 화합물

생성물 1

HCID 69367981HCID 69367981, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

A solution of 2-(benzhydrylideneamino)-5-(4-methoxy-2,3-dimethylphenyl)-5-oxopentanoic acid ethyl ester (16.56 mmol) in EtOH (80 mL) containing 10% Pd/C (760 mg) is stirred under an atmosphere of H2 (double-stuffed balloon) for 18 h. The reaction mixture is then filtered through of pad of Celite using MeOH for the rinse. The filtrated is concentrated in vacuo to a nearly colorless syrup, which is used in the next reaction without further purification. 1H NMR (CDCl3, 400 MHz): 7.46 (d, J=8.6 Hz, 1H), 6.75 (d, J=8.6 Hz, 1H), 4.40 (dd, J=8.8, 6.6 Hz, 1H), 4.23 (q, J=8.8 Hz, 2H), 3.90 (dd, J=8.6, 5.4 Hz, 1H), 3.82 (s, 3H), 2.29 (s, 3H), 2.19 (s, 3H), 2.25-2.05 (m, 4H), 1.72-1.65 (m, 1H), 1.31 (t, J=8.8 Hz, 3H). Electrospray MS: m/z 278 [M+1].

후처리

  1. filtrationThe reaction mixture is then filtered through of pad of Celite
  2. concentrationThe filtrated is concentrated in vacuo to a nearly colorless syrup, which
  3. customis used in the next reaction without further purification

출처 및 근거

ORD 기록
ord-b8efd55456444ec7b775b93dadec994b
출처 데이터셋
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07253168B2

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