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HCID 67581870, 화합물 → HCID 57011354, 화합물

HRID 1416479
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HRID 1416479 반응식
C(OC([N:11]1[CH2:16][CH2:15][N:14]([C:17]2[N:26]=[C:25]([O:27][C@@H:28]3[CH2:32][C@H:31]([O:33][CH3:34])[C@@H:30]([OH:35])[C@H:29]3[OH:36])[C:24]3[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=3)[N:18]=2)[CH2:13][CH2:12]1)=O)C1C=CC=CC=1>CO.[Pd]>[OH:36][C@@H:29]1[C@H:30]([OH:35])[C@@H:31]([O:33][CH3:34])[CH2:32][C@H:28]1[O:27][C:25]1[C:24]2[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=2)[N:18]=[C:17]([N:14]2[CH2:13][CH2:12][NH:11][CH2:16][CH2:15]2)[N:26]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 67581870HCID 67581870, 화합물

생성물 1

HCID 57011354HCID 57011354, 화합물수율 75%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

To a solution of 2-[4-(benzyloxycarbonyl)piperazin-1-yl]-4-[(1R,2R,3S,4S)-(2,3-dihydroxy-4-methoxycyclopentan-1-yl)oxy]quinazoline (5.40 g) in methanol (108 ml) is added 10% palladium/carbon (1.00 g), and the mixture is stirred under hydrogen atmosphere and under atmospheric pressure at room temperature for 16.5 hours. The reaction mixture is filtered, and the filtrate is evaporated to dryness under reduced pressure, and the residue is crystallized from diethyl ether to give 4-[(1R,2R,3S,4S)-(2,3-dihydroxy-4-methoxycyclopentan-1-yl)oxy]-2-(1-piperazinyl)quinazoline (2.95 g) as crystals. A part of this product is recrystallized from ethanol-diethyl ether to give a pure crystalline product, which has the following physical properties.

후처리

  1. filtrationThe reaction mixture is filtered
  2. customthe filtrate is evaporated to dryness under reduced pressure
  3. customthe residue is crystallized from diethyl ether

출처 및 근거

ORD 기록
ord-b77b0e29b42c41ff9c75ea34f2dfdf80
출처 데이터셋
uspto-grants-1999_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05912247

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