HCID 67582830, 화합물 → HCID 54302338, 화합물

HRID 1416491노트

반응식

HRID 1416491 반응식
C(OC([N:11]1[CH2:16][CH2:15][N:14]([C:17]2[N:26]=[C:25]([O:27][CH2:28][CH:29]([OH:33])[CH:30]([OH:32])[CH3:31])[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:33][CH:29]([CH:30]([OH:32])[CH3:31])[CH2:28][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 물질

4

반응물 1

HCID 67582830HCID 67582830, 화합물

생성물 1

HCID 54302338HCID 54302338, 화합물수율 35.2%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

To a solution of 2-[4-(benzyloxycarbonyl)piperazin-1-yl]-4-[(2RS,3RS)-(2,3-dihydroxybutan-1-yl)oxy]quinazoline (950 mg) in methanol (21 ml) is added 10% palladium/carbon (109 mg), and the mixture is stirred under hydrogen atmosphere and under atmospheric pressure at room temperature for 8 hours. The reaction mixture is filtered, and the filtrate is evaporated to dryness under reduced pressure, and the residue is crystallized from acetone-diethyl ether. The crystals thus obtained are recrystallized from ethanol - diethyl ether to give 4-[(2RS,3RS)-(2,3-dihydroxybutan-1-yl)oxy]-2-(1-piperazinyl)quinazoline (235 mg) as crystals.

후처리

  1. filtrationThe reaction mixture is filtered
  2. customthe filtrate is evaporated to dryness under reduced pressure
  3. customthe residue is crystallized from acetone-diethyl ether
  4. customThe crystals thus obtained
  5. customare recrystallized from ethanol - diethyl ether

출처 및 근거

ORD 기록
ord-1a412b68e070493b803f1d778569d1cc
출처 데이터셋
uspto-grants-1999_06
특허 번호
US05912247

반응 노트

불러오는 중…