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Methanol → HCID 11955818, 화합물

HRID 644687
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HRID 644687 반응식
C([O:8][C:9]1[CH:14]=[C:13]([O:15]CC2C=CC=CC=2)[C:12]([C:23]([CH3:25])=[CH2:24])=[CH:11][C:10]=1[C:26]([N:28]1[CH2:36][C:35]2[C:30](=[CH:31][CH:32]=[C:33]([O:37][CH2:38][CH2:39][N:40]([CH3:42])[CH3:41])[CH:34]=2)[CH2:29]1)=[O:27])C1C=CC=CC=1.[CH3:43]O>[Pd]>[OH:8][C:9]1[CH:14]=[C:13]([OH:15])[C:12]([CH:23]([CH3:24])[CH3:25])=[CH:11][C:10]=1[C:26]([N:28]1[CH2:36][C:35]2[C:30](=[C:31]([CH3:43])[CH:32]=[C:33]([O:37][CH2:38][CH2:39][N:40]([CH3:42])[CH3:41])[CH:34]=2)[CH2:29]1)=[O:27]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 887MethanolHCID 46916064(2,4-Bis-benzyloxy-5-isopropenyl-phenyl)-[5-(2-dimethylamino-ethoxy)-1,3-dihydro-isoindol-2-yl]-methanone

생성물 1

HCID 11955818HCID 11955818, 화합물수율 35%

시약·촉매·용매 1

HCID 23938Palladium촉매

실험 절차

(2,4-Bis-benzyloxy-5-isopropenyl-phenyl)-[5-(2-dimethylamino-ethoxy)-1,3-dihydro-isoindol-2-yl]-methanone (37 mg, 0.06 mmol) was hydrogenated in methanol at 50° C. over 10% palladium on charcoal using an H-cube hydrogenation apparatus, under free hydrogen conditions. The product was purified by preparative HPLC (basic method) to give the title compound as an off-white solid (9 mg, 35%). 1H NMR (MeOH-d4) 7.18 (1H, s), 6.77-6.65 (2H, br.m), 6.37 (1H, s), 4.85 (water obscuring CH2), 4.77 (2H, s), 4.08 (2H, t), 3.20 (1H, sept), 2.81 (2H, t), 2.39 (6H, s), 2.22 (3H, br.s), 1.21 (6H, d). MS: [M+H]+ 399.

후처리

  1. customThe product was purified by preparative HPLC (basic method)

출처 및 근거

ORD 기록
ord-8c9be4c25122408095b553db30f9e1b0
출처 데이터셋
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07700625B2

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