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Di-tert-butyl dicarbonate → HCID 131720448、化合物

HRID 727719
ノート
印刷プレビュー

反応式

HRID 727719 の反応式
[S:1]([OH:5])([OH:4])(=[O:3])=[O:2].[C:6]([N:9]1[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]1)(=[NH:8])[NH2:7].[C:15]([N:18]1[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]1)(=[NH:17])[NH2:16].[C:24](O[C:32]([O:34][C:35]([CH3:38])([CH3:37])[CH3:36])=[O:33])([O:26][C:27]([CH3:30])([CH3:29])[CH3:28])=[O:25]>O1CCCC1.O>[S:1]([OH:5])([OH:4])(=[O:3])=[O:2].[C:6]([N:9]1[CH2:14][CH2:13][N:12]([C:24]([O:26][C:27]([CH3:30])([CH3:29])[CH3:28])=[O:25])[CH2:11][CH2:10]1)(=[NH:7])[NH2:8].[C:15]([N:18]1[CH2:23][CH2:22][N:21]([C:32]([O:34][C:35]([CH3:36])([CH3:37])[CH3:38])=[O:33])[CH2:20][CH2:19]1)(=[NH:16])[NH2:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 90495Di-tert-butyl dicarbonateHCID 448907111-Piperazinecarboximidamide, sulfate (2:1)

生成物 1

HCID 131720448HCID 131720448、化合物収率 63.4%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒2 回

実験手順

2.50 g of 1-amidinopiperazine hemisulfate were dissolved in 60 ml of a 1:1 by volume mixture of tetrahydrofuran and water, and a solution of 3.40 g of di-t-butyl dicarbonate in 10 ml of tetrahydrofuran was added to the resulting solution, after which the mixture was stirred at room temperature for 2.5 hours. At the end of this time, the tetrahydrofuran was removed from the reaction mixture by distillation under reduced pressure, the insolubles were filtered off and the filtrate was evaporated to dryness under reduced pressure. The resulting residue was extracted with ethanol (twice, each time with 50 ml). and methanol (twice, each time with 50 ml). The extract was evaporated to dryness to obtain 2.48 g of the title compound, as crystals, melting at 278° C. (with decomposition).

後処理

  1. customAt the end of this time, the tetrahydrofuran was removed from the reaction mixture by distillation under reduced pressure
  2. filtrationthe insolubles were filtered off
  3. customthe filtrate was evaporated to dryness under reduced pressure
  4. extractionThe resulting residue was extracted with ethanol (twice, each time with 50 ml)
  5. customThe extract was evaporated to dryness

出典と根拠

ORDレコード
ord-7c07c59303bc405e8ece3862fa604c97
出典データセット
uspto-grants-1998_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05712267

反応ノート

読み込み中…

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