Triethylamine → HCID 67582976, 화합물

HRID 1416489노트

반응식

HRID 1416489 반응식
[CH2:1]([O:5][C:6]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[N:9]=[C:8]([N:16]2[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]2)[N:7]=1)/[CH:2]=[CH:3]/[CH3:4].C(N(CC)CC)C.[C:29](Cl)(=[O:38])[O:30][CH2:31][C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1>C(Cl)Cl.C(Cl)(Cl)Cl>[CH2:31]([O:30][C:29]([N:19]1[CH2:20][CH2:21][N:16]([C:8]2[N:7]=[C:6]([O:5][CH2:1]/[CH:2]=[CH:3]/[CH3:4])[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[N:9]=2)[CH2:17][CH2:18]1)=[O:38])[C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 10387Benzyl chloroformateHCID 67582001HCID 67582001, 화합물

생성물 1

HCID 67582976HCID 67582976, 화합물

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 6344Dichloromethane용매2회

실험 절차

To a solution of 4-[trans-(2-buten-1-yl)oxy]-2-(1-piperazinyl) quinazoline (1.20 g) in dry methylene chloride (12 ml) is added triethylamine (1.77 ml) with stirring under ice-cooling, and thereto is further added dropwise a solution of benzyl chlorocarbonate (0.73 ml) in dry methylene chloride (5 ml). The mixture is stirred under ice-cooling for 3 hours. The reaction mixture is diluted with chloroform, washed with water, and dried over anhydrous magnesium sulfate. The solution is evaporated to dryness under reduced pressure, and the residue is purified by medium pressure liquid column chromatography (elutant, chloroform) to give 2-[4-(benzyloxycarbonyl)piperazin-1-yl]-4-[trans-(2-buten-1-yl)oxy]quinazoline (1.57 g) as crystals.

후처리

  1. temperaturecooling
  2. stirringThe mixture is stirred under ice-
  3. temperaturecooling for 3 hours
  4. washwashed with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customThe solution is evaporated to dryness under reduced pressure
  7. customthe residue is purified by medium pressure liquid column chromatography (elutant, chloroform)

출처 및 근거

ORD 기록
ord-b65bdff6da5e487d859ecf4fbd1bbdc7
출처 데이터셋
uspto-grants-1999_06
특허 번호
US05912247

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