Triethylamine → HCID 67582976、化合物

HRID 1416489ノート

反応式

HRID 1416489 の反応式
[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

参加物

6

反応物 3

HCID 8471TriethylamineHCID 10387Benzyl chloroformateHCID 67582001HCID 67582001、化合物

生成物 1

HCID 67582976HCID 67582976、化合物

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 6344Dichloromethane溶媒2 回

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-b65bdff6da5e487d859ecf4fbd1bbdc7
出典データセット
uspto-grants-1999_06
特許番号
US05912247

反応ノート

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